183 results on '"Inductively coupled plasma"'
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2. Natural silicate nanoparticles: separation, characterization, and assessment of stability and perspectives of their use as reference nanomaterials
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Natalia N. Fedyunina, Petr S. Fedotov, A. I. Ivaneev, V. K. Karandashev, Mikhail S. Ermolin, and Andrey A. Burmistrov
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Materials science ,Muscovite ,010401 analytical chemistry ,Atomic emission spectroscopy ,Nanoparticle ,02 engineering and technology ,engineering.material ,021001 nanoscience & nanotechnology ,01 natural sciences ,Biochemistry ,0104 chemical sciences ,Analytical Chemistry ,Nanomaterials ,chemistry.chemical_compound ,Montmorillonite ,Chemical engineering ,Dynamic light scattering ,chemistry ,engineering ,Kaolinite ,Inductively coupled plasma ,0210 nano-technology - Abstract
Natural nanomaterials, which play a very important role in environmental processes, are so far poorly studied. Firstly, the separation of nanoparticles from the bulk sample is a challenge. Secondly, the absence of reference natural nanomaterials makes it impossible to compare the results obtained by different researchers and develop a unified methodology for the separation and characterization of natural nanomaterials. Therefore, the development of reference natural nanomaterials is an urgent need of the environmental analytical chemistry. In this work, mineral nanoparticles (kaolinite, montmorillonite, muscovite, and quartz) have been studied as potential reference natural nanomaterials. A set of analytical methods including coiled-tube field-flow fractionation, scanning electron microscopy, dynamic light scattering, laser diffraction, inductively coupled plasma atomic emission, and mass spectrometry are applied to the separation and characterization of nanoparticles. It has been shown by laser diffraction that 93–98% of separated mineral nanoparticles are in the size range from about 40 to 300 nm, while 2–7% have size up to 830 nm. The size range of particles is confirmed by electron microscopy. Major (Al, Na, K, Ca, Fe), trace (Ti, Co, Cu, Zn, Tl, Pb, Bi, etc.), and rare earth elements have been determined in the suspensions of kaolinite, montmorillonite, and muscovite nanoparticles. Based on Al content, the concentration of mineral nanoparticles in suspensions is estimated. Agglomeration stability (consistency of size distribution) of nanoparticles at pH 6–8 is assessed. It has been shown that muscovite nanoparticles are stable at pH 7–8, whereas montmorillonite nanoparticles are stable only at pH 8 for at least 4 weeks. A noticeable agglomeration of kaolinite nanoparticles is observed at pH 6–8. Due to the low concentration of quartz nanoparticles, their characterization and stability assessment are hindered. The challenges of the development of reference natural nanomaterials are discussed.
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- 2021
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3. Sweat chloride assay by inductively coupled plasma mass spectrometry: a confirmation test for cystic fibrosis diagnosis
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Marvelli, Antonella, Campi, Beatrice, Mergni, Gianfranco, Di Cicco, Maria Elisa, Turini, Paola, Scardina, Paolo, Zucchi, Riccardo, Pifferi, Massimo, Taccetti, Giovanni, Paolicchi, Aldo, la Marca, Giancarlo, and Saba, Alessandro
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- 2020
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4. Modeling plasmas in analytical chemistry—an example of cross-fertilization
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Bogaerts, Annemie
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- 2020
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5. Hanging drop cathode-atmospheric pressure glow discharge as a new method of sample introduction for inductively coupled plasma-optical emission spectrometry
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Swiderski, Krzysztof, Welna, Maja, Greda, Krzysztof, Pohl, Pawel, and Jamroz, Piotr
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- 2020
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6. Sweat chloride assay by inductively coupled plasma mass spectrometry: a confirmation test for cystic fibrosis diagnosis
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Beatrice Campi, Giovanni Taccetti, Alessandro Saba, Giancarlo la Marca, G. Mergni, Paola Turini, Paolo Scardina, Massimo Pifferi, Maria Di Cicco, Antonella Marvelli, Riccardo Zucchi, and Aldo Paolicchi
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Adult ,030213 general clinical medicine ,Cystic fibrosis, Inductively coupled plasma, Mass spectrometry, Chloride assay ,Cystic Fibrosis ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Chloride ,Cystic fibrosis ,Chloride assay ,Analytical Chemistry ,SWEAT ,Coulometry ,03 medical and health sciences ,0302 clinical medicine ,Chlorides ,Limit of Detection ,medicine ,Humans ,Sweat ,Inductively coupled plasma mass spectrometry ,Detection limit ,Chromatography ,Chemistry ,010401 analytical chemistry ,Reproducibility of Results ,Middle Aged ,medicine.disease ,0104 chemical sciences ,Case-Control Studies ,Inductively coupled plasma ,Research Paper ,medicine.drug - Abstract
The current guidelines for sweat chloride analysis identify the procedures for sweat collection, but not for chloride assay, which is usually performed by methods originally not aiming at the low concentrations of chloride found in sweat. To overcome this limitation, we set up, characterized, and adopted an original inductively coupled plasma mass spectrometry (ICP-MS) method for sweat chloride determination, which was designed for its easy use in a clinical laboratory. The method was linear in the range 8.5E−3 to 272.0E−3 mM, precision exhibited a relative standard deviation
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- 2020
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7. Determination of halogens and sulfur in honey: a green analytical method using a single analysis
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Priscila Tessmer Scaglioni, Mariele S. Nascimento, Fernanda P. Balbinot, Rochele S. Picoloto, Marcia F. Mesko, and Vanize C. Costa
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Analyte ,Chemistry ,010401 analytical chemistry ,Ion chromatography ,Analytical chemistry ,02 engineering and technology ,Standard solution ,021001 nanoscience & nanotechnology ,Mass spectrometry ,01 natural sciences ,Biochemistry ,0104 chemical sciences ,Analytical Chemistry ,Halogen ,Sample preparation ,Inductively coupled plasma ,0210 nano-technology ,Inductively coupled plasma mass spectrometry - Abstract
The halogen determination is important in view of their biological and environmental roles, but their determination has still been considered a challenge, especially at low concentrations. Therefore, a method for honey decomposition using microwave-induced combustion (MIC) combined with ion chromatography and conductimetric detection (for Cl, F, and S determination) or mass detection (for Br and I determination) (IC-CD-MS) is proposed. Trueness was evaluated by adding reference materials (RMs) or a standard solution in the sample. By using 50 mmol L−1 NH4OH as the absorbing solution, recoveries for all analytes were between 94 and 103%, in both tests. Moreover, no statistical difference (t test, confidence level of 95%) was observed for the results obtained by IC in comparison with those obtained by inductively coupled plasma optical emission spectroscopy (Cl and S) and by inductively coupled plasma mass spectrometry (Br and I). Finally, the proposed method was applied to 19 honey samples from different origins. The concentrations ranged from
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- 2020
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8. Selective pressurized hot water extraction of nutritious macro-nutrients vs. micro-nutrients in Moringa oleifera leaves—a chemometric approach
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Luke Chimuka, Said Al-Hamimi, Hlanganani Tutu, Charlotta Turner, Ewa Cukrowska, Phatsimo G. Matshediso, and Yannick Nuapia
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Hot Temperature ,02 engineering and technology ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,Moringa ,Pressure ,Food science ,Response surface methodology ,Moringa oleifera ,Plant Extracts ,Macro nutrients ,Chemistry ,010401 analytical chemistry ,Extraction (chemistry) ,Water ,Nutrients ,Elements ,021001 nanoscience & nanotechnology ,Micronutrient ,0104 chemical sciences ,Plant Leaves ,Hot water extraction ,Optical emission spectroscopy ,Inductively coupled plasma ,0210 nano-technology - Abstract
Moringa oleifera leaves are widely used in traditional medicine as a food supplement because they are high in essential and nutritious content. Pressurized hot water extraction (PHWE), which is a green approach, was used for the recovery of the macro-nutrient and micro-nutrient elements from dried leaf powder of Moringa oleifera. In this study, response surface methodology was applied to assess the influence of temperature (50-200 °C) and time (5-60 min) on the extractability pattern of macro-nutrient and micro-nutrient elements from the leaves of Moringa oleifera when processed by PHWE. The quantification of macro-nutrient elements such as Ca, K and Mg and micro-nutrient elements like Al, Co, Cr, Cu, Fe, Ni and Zn from the leaves was determined using inductively coupled plasma optical emission spectroscopy (ICP-OES). Obtained results revealed that the extraction of macro-nutrient elements from the Moringa oleifera leaves was enhanced by increasing the extraction time more than the extraction temperature. On the contrary, the amounts of extractable micro-nutrient elements were increased by increasing the extraction temperature. Hence, the recovery for macro-nutrient elements ranged from 88 to 98% while for micro-nutrients it ranged from 21 to 46%. This implies that macro-nutrient elements are extracted with relatively high selectivity in relation to micro-nutrient elements in Moringa dried leaf powder using the PHWE technique.
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- 2020
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9. Single analysis of human hair for determining halogens and sulfur after sample preparation based on combustion reaction
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Priscila Tessmer Scaglioni, Rodrigo Mendes Pereira, Marcia F. Mesko, and Diogo La Rosa Novo
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02 engineering and technology ,Standard solution ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Mass Spectrometry ,Analytical Chemistry ,Halogens ,Humans ,Sample preparation ,Inductively coupled plasma mass spectrometry ,Chromatography ,integumentary system ,Chemistry ,010401 analytical chemistry ,Hair analysis ,Electric Conductivity ,Reproducibility of Results ,Repeatability ,Reference Standards ,021001 nanoscience & nanotechnology ,0104 chemical sciences ,Inductively coupled plasma atomic emission spectroscopy ,Feasibility Studies ,Inductively coupled plasma ,0210 nano-technology ,Pyrolysis ,Sulfur ,Hair - Abstract
A single analysis of hair for determining halogens (chlorine, bromine, fluorine, and iodine) and sulfur by ion chromatography with suppressed conductivity and mass spectrometry detection (IC-MS) was proposed. Inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) were also used to compare the results. For this purpose, 300 mg of human hair were digested by microwave-induced combustion (MIC) using 20 bar of oxygen pressure. The analytes were absorbed in 100 mmol L−1 NH4OH. Trueness of the proposed method was evaluated by analysis of a CRM of human hair; by recovery tests, using standard solution at two levels (50% and 100%), and by comparison of results with those obtained by ICP OES (Cl and S) and ICP-MS (Br and I). Suitable recoveries (ranging from 92 to 105%) were obtained, and the results from CRM analysis did not differ significantly from those described in the certificate. Moreover, results obtained by IC-MS did not present significant differences (p > 0.05) from those obtained by ICP OES and by ICP-MS. Precision was evaluated in terms of repeatability and intermediate precision, and the relative standard deviations were always lower than 8%. The proposed method presented good accuracy and it is a reliable strategy for human hair analysis. Final digests obtained using the MIC method were fully compatible with all proposed determination techniques. Compared to others reported in the literature, the proposed method presents several advantages, especially given that it is possible to determine halogens and sulfur in a single analysis.
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- 2019
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10. Hanging drop cathode-atmospheric pressure glow discharge as a new method of sample introduction for inductively coupled plasma-optical emission spectrometry
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Krzysztof Greda, Piotr Jamroz, Maja Welna, Krzysztof Swiderski, and Pawel Pohl
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Glow discharge ,Materials science ,Atmospheric pressure ,Drop (liquid) ,Communication ,Analytical chemistry ,Atmospheric pressure glow discharge ,Alkali metal ,Optical emission spectrometry ,Biochemistry ,Cathode ,Analytical Chemistry ,law.invention ,Transition metal ,law ,Sample introduction ,Emission spectrum ,Hanging drop cathode ,Inductively coupled plasma - Abstract
This work reports the use of hanging drop cathode-atmospheric pressure glow discharge (HDC-APGD) as a new method of sample introduction for inductively coupled plasma-optical emission spectrometry (ICP-OES). The developed arrangement was characterized by a low sample uptake (0.56 mL min−1) and the fact that the entire sample solution volume was consumed by the discharge. This resulted in a very high transport efficiency of analytes from the sample solution into the ICP torch (usually > 80%). Under the optimal operating conditions of HDC-APGD, intensities of emission lines of studied elements were, on average, 2 times higher as compared to those obtained with conventional pneumatic nebulization (PN). Moreover, in the case of I and Y, the observed signal enhancements were even higher, i.e., 6.2 and 6.1 times, respectively. It was also shown that in the case of B and some elements that are known to form different volatile species (Ag, Bi, Cd, Hg, Os, Pb, and Se), the presence of low molecular weight organic compounds in the sample solution, i.e., CH3OH, C2H5OH, HCOOH, CH3COOH, or HCHO, resulted in the additional enhancement of their signals. It was especially evident in the case of Hg for which a 8.6-fold signal enhancement in the presence of HCOOH was noticed. The system presented herein was distinguished from other competitive APGD-type discharges because it could be successfully used for the determination of a vast group of elements, including alkali metals, alkaline earth metals, transition metals, and non-metals. Electronic supplementary material The online version of this article (10.1007/s00216-020-02685-7) contains supplementary material, which is available to authorized users.
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- 2020
11. Determination of 107Pd in Pd purified by selective precipitation from spent nuclear fuel by laser ablation ICP-MS
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Takumi Yomogida, Takuma Horita, Masaki Ohata, Yukiko Hanzawa, Hironori Ohba, Shiho Asai, Morihisa Saeki, and Yoshihiro Kitatsuji
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Laser ablation ,Materials science ,Precipitation (chemistry) ,010401 analytical chemistry ,Analytical chemistry ,02 engineering and technology ,021001 nanoscience & nanotechnology ,Mass spectrometry ,01 natural sciences ,Biochemistry ,0104 chemical sciences ,Analytical Chemistry ,Dilution ,chemistry.chemical_compound ,chemistry ,Aqua regia ,Inductively coupled plasma ,0210 nano-technology ,Inductively coupled plasma mass spectrometry ,Dissolution - Abstract
Determination of radiopalladium 107Pd is required to ensure radiation safety of the Pd extracted from spent nuclear fuel for recycling or disposal. We employed nanosecond laser ablation inductively coupled plasma quadrupole mass spectrometry (ns-LA-ICP-QMS) to simplify the analytical procedure of 107Pd. Pd was separated through a selective Pd precipitation reaction induced by pulsed laser irradiation that reduces Pd(II) ions to metal Pd(0). Laser ablation facilitates direct measurement of the Pd precipitates, skipping the dissolution and dilution procedure with aqua regia and HCl, which causes serious corrosion damage to the introduction system of the ICP. In the present study, 102Pd in natural Pd standard solution was used as an internal standard owing to its absence in spent nuclear fuel. Pd precipitates with diameters ranging from 0.2 to 0.5 μm, obtained by pulsed laser irradiation, were embedded uniformly on the surface of the centrifugal filter to form a microscopically thin and flat Pd surface. The resulting homogeneous Pd layer is suitable for obtaining a stable signal ratio of 107Pd/102Pd (
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- 2018
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12. Improving the reliability of the iron concentration quantification for iron oxide nanoparticle suspensions: a two-institutions study
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Cordula Grüttner, M. Puerto Morales, Rocío Costo, Nicole Gehrke, David Heinke, Fritz Westphal, and Sabino Veintemillas-Verdaguer
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Iron analyses ,Materials science ,Iron oxide ,02 engineering and technology ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,Iron oxide nanoparticles ,chemistry.chemical_compound ,Colorimetric analysis ,Spectrophotometry ,medicine ,Sample preparation ,Dissolution ,Inductively coupled plasma analysis ,Chromatography ,medicine.diagnostic_test ,010401 analytical chemistry ,021001 nanoscience & nanotechnology ,Inter-institutional study ,0104 chemical sciences ,Dilution ,chemistry ,Comparative study ,Inductively coupled plasma ,0210 nano-technology ,Research Paper - Abstract
Most iron oxide nanoparticles applications, and in special biomedical applications, require the accurate determination of iron content as the determination of particle properties from measurements in dispersions is strongly dependent on it. Inductively coupled plasma (ICP) and spectrophotometry are two typical worldwide used analytical methods for iron concentration determination. In both techniques, precise determination of iron is not straightforward and nanoparticle digestion and dilution procedures are needed prior to analysis. The sample preparation protocol has been shown to be as important as the analytical method when accuracy is aimed as many puzzling reported results in magnetic, colloidal, and structural properties are simply attributable to inadequate dissolution procedures. Therefore, a standard sample preparation protocol is needed to ensure the adequate and complete iron oxide nanoparticle dissolution and to harmonize this procedure. In this work, an interlaboratory evaluation of an optimized iron oxide nanoparticle digestion/dilution protocol was carried out. The presented protocol is simple, inexpensive, and does not involve any special device (as microwave, ultrasound, or other high-priced digestion devices). Then, iron concentration was measured by ICP-OES (performed in ICMM/CSIC-Spain) and spectrophotometry (NanoPET-Germany) and the obtained concentration values were analyzed to determine the most probable error causes. Uncertainty values as low as 1.5% were achieved after the optimized method was applied. Moreover, this article provides a list of recommendations to significantly reduce uncertainty in both sample preparation and analysis procedures. Graphical abstract ᅟ.
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- 2018
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13. Multielement analysis of Zanthoxylum bungeanum Maxim. essential oil using ICP-MS/MS
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Hualin Xie, Liang Fu, and Shuyun Shi
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Zanthoxylum ,Vapor pressure ,Tandem mass spectrometry ,01 natural sciences ,Biochemistry ,Arsenic ,Analytical Chemistry ,0404 agricultural biotechnology ,Tandem Mass Spectrometry ,Oils, Volatile ,Skimmer (machine) ,Inductively coupled plasma mass spectrometry ,Detection limit ,Chromatography ,Chemistry ,010401 analytical chemistry ,Extraction (chemistry) ,Mercury ,04 agricultural and veterinary sciences ,040401 food science ,Trace Elements ,0104 chemical sciences ,Dilution ,Lead ,Inductively coupled plasma ,Cadmium - Abstract
The concentrations of trace elements (Cr, Ni, As, Cd, Hg, and Pb) in Zanthoxylum bungeanum Maxim. essential oil (ZBMEO) were determined by inductively coupled plasma tandem mass spectrometry. The ZBMEO sample was directly analyzed after simple dilution with n-hexane. Aiming for a relatively high vapor pressure of n-hexane and its resultant loading on plasma, we used a narrow injector torch and optimized plasma radio frequency power and carrier gas flow to ensure stable operation of the plasma. An optional gas flow of 20% O2 in Ar was added to the carrier gas to prevent the incomplete combustion of highly concentrated organic carbon in plasma and the deposition of carbon on the sampling and skimmer cone orifices. In tandem mass spectrometry mode, O2 was added to the collision/reaction cell to eliminate the interferences. The limits of detection for Cr, Ni, As, Cd, Hg, and Pb were 2.26, 1.64, 2.02, 1.35, 1.76, and 0.97 ng L-1, respectively. After determination of 23 ZBMEO samples from different regions in China, we found that the average concentration ranges of trace elements in the 23 ZBMEO samples were 0.72-6.02 ng g-1, 0.09-2.87 ng g-1, 0.21-5.84 ng g-1, 0.16-2.15 ng g-1, 0.13-0.92 ng g-1, and 0.17-0.73 ng g-1 for Cr, Ni, As, Cd, Hg, and Pb, respectively. The trace elements in ZBMEO differed significantly when different extraction technologies were used. The study revealed that the contents of the toxic elements As, Cd, Hg, and Pb were extremely low, and hence they are unlikely to pose a health risk following ZBMEO ingestion. Graphical abstract The working mechanism of sample analysis by ICP-MS/MS.
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- 2018
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14. Aptamer-facilitated mass cytometry
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Olga Loboda, Gleb G. Mironov, Jessica Watson, Maxim V. Berezovski, Olga Ornatsky, and Alexandre Bouzekri
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0301 basic medicine ,Lymphoblastic Leukemia ,Aptamer ,Mass spectrometry ,Biochemistry ,Mass Spectrometry ,Analytical Chemistry ,Flow cytometry ,03 medical and health sciences ,0302 clinical medicine ,Cell Line, Tumor ,medicine ,Humans ,Biotinylation ,Mass cytometry ,Chromatography ,biology ,medicine.diagnostic_test ,Chemistry ,Receptor Protein-Tyrosine Kinases ,NeutrAvidin ,Aptamers, Nucleotide ,Precursor Cell Lymphoblastic Leukemia-Lymphoma ,Avidin ,Flow Cytometry ,Burkitt Lymphoma ,030104 developmental biology ,030220 oncology & carcinogenesis ,biology.protein ,Inductively coupled plasma ,Cell Adhesion Molecules - Abstract
Mass cytometry is a novel cell-by-cell analysis technique, which uses elemental tags instead of fluorophores. Sample cells undergo rapid ionization in inductively coupled plasma and the ionized elemental tags are then analyzed by means of time-of-flight mass spectrometry. Benefits of the mass cytometry approach are in no need for compensation, the high number of detection channels (up to 100) and low background noise. In this work, we applied a biotinylated aptamer against human PTK7 receptor for characterization of positive (human acute lymphoblastic leukemia) and negative (human Burkitt's lymphoma) cells by a mass cytometry instrument. Our proof of principal experiments showed that biotinylated aptamers in conjunction with metal-labeled neutravidin can be successfully utilized for mass cytometry experiments at par with commercially available antibodies. Graphical abstract Biotinylated aptamers in conjunction with metal-labeled neutravidin bind to cell biomarkers, and then injected into the inductively coupled plasma (ICP) source, where cells are vaporized, atomized, and ionized in the plasma for subsequent mass spectrometry (MS) analysis of lanthanide metals.
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- 2018
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15. Quantification of elemental area densities in multiple metal layers (Au/Ni/Cu) on a Cr-coated quartz glass substrate for certification of NMIJ CRM 5208-a
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Toshiko Takatsuka, Yanbei Zhu, Akira Kurokawa, Tomoko Ariga, Kazumi Inagaki, Mika Ito, and Shinya Terauchi
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010302 applied physics ,Materials science ,Scanning electron microscope ,010401 analytical chemistry ,Analytical chemistry ,Substrate (electronics) ,01 natural sciences ,Biochemistry ,0104 chemical sciences ,Analytical Chemistry ,Certified reference materials ,0103 physical sciences ,Area density ,Inductively coupled plasma ,Quartz ,Layer (electronics) ,Inductively coupled plasma mass spectrometry - Abstract
Area densities of Au/Ni/Cu layers on a Cr-coated quartz substrate were characterized to certify a multiple-metal-layer certified reference material (NMIJ CRM5208-a) that is intended for use in the analysis of the layer area density and the thickness by an X-ray fluorescence spectrometer. The area densities of Au/Ni/Cu layers were calculated from layer mass amounts and area. The layer mass amounts were determined by using wet chemical analyses, namely inductively coupled plasma mass spectrometry (ICP-MS), isotope-dilution (ID-) ICP-MS, and inductively coupled plasma optical emission spectrometry (ICP-OES) after dissolving the layers with diluted mixture of HCl and HNO3 (1:1, v/v). Analytical results of the layer mass amounts obtained by the methods agreed well with each another within their uncertainty ranges. The area of the layer was determined by using a high-resolution optical scanner calibrated by Japan Calibration Service System (JCSS) standard scales. The property values of area density were 1.84 ± 0.05 μg/mm2 for Au, 8.69 ± 0.17 μg/mm2 for Ni, and 8.80 ± 0.14 μg/mm2 for Cu (mean ± expanded uncertainty, coverage factor k = 2). In order to assess the reliability of these values, the density of each metal layer calculated from the property values of the area density and layer thickness measured by using a scanning electron microscope were compared with available literature values and good agreement between the observed values and values obtained in previous studies.
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- 2018
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16. Fully automated focused infrared microashing combined with use of ICP-based instruments for rapid analysis of multiple elements in biological samples
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Zhang, Ni and Zheng, Jianbin
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- 2017
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17. Fully automated focused infrared microashing combined with use of ICP-based instruments for rapid analysis of multiple elements in biological samples
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Ni Zhang and Jianbin Zheng
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Hot Temperature ,Time Factors ,Materials science ,Infrared Rays ,Analytical chemistry ,02 engineering and technology ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,Automation ,Sample preparation ,Infrared heater ,Dissolution ,Inductively coupled plasma mass spectrometry ,Carbonization ,010401 analytical chemistry ,021001 nanoscience & nanotechnology ,Trace Elements ,0104 chemical sciences ,Certified reference materials ,Ashing ,Biological Assay ,Metals, Rare Earth ,Inductively coupled plasma ,0210 nano-technology ,Oxidation-Reduction - Abstract
A fully automated focused infrared microashing sample preparation system was proposed for preparation of biological samples with high organic matter content for the determination of multiple elements combined with inductively coupled plasma optical emission spectroscopy and inductively coupled plasma mass spectrometry. The whole ashing procedure, including sample transfer, carbonization and oxidation of the sample, dissolution of ash, constant volume control, and homogenization of the solution, was automatically controlled. Gold-plated infrared tubes were used to produce and focus infrared radiation to heat the sample. Ozone was used to accelerate the carbonization of samples at a lower temperature to avoid the production of large amounts of empyreumatic oil. In addition, the self-designed double-layer tube serves as a site for ashing and carbonization of the sample and as a container for dissolving ash, as well as for holding the solution. This is the only container in the entire system to reduce the risk of pollution. Eight biological certified reference materials were used as examples to evaluate the performance of the proposed device. A sample ashing pretreatment cycle, from solid sample to liquid solution, took only 40 min and simultaneously treated 12 samples. Except for individual results, the relative errors between the certified values and recorded values for 38 micro and trace elements, including Ca, Mg, Na, P, Li, Be, Sc, Ti, V, Mn, Co, Ni, Cu, Zn, Rb, Sr, Y, Mo, Ag, Cs, Ba, Tl, Th, U, and rare earth elements, were typically less than 30%. The relative standard deviations for five determinations were typically less than 15%. Graphical abstract Automated dry ashing sample preparation system. ICP inductively coupled plasma.
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- 2017
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18. An 'on-off-on' fluorescent probe for ascorbic acid based on Cu-ZnCdS quantum dots and α-MnO2 nanorods
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Xianying Zeng, Hua He, Hongwei Ge, Wei Liu, Zhaoyi Zhang, Ping Zou, Xin Liu, Yaqin Liu, Hanbing Rao, Yanying Wang, Xianxiang Wang, Yao Gao, and Yan Yang
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Materials science ,Analytical chemistry ,02 engineering and technology ,010402 general chemistry ,021001 nanoscience & nanotechnology ,Ascorbic acid ,01 natural sciences ,Biochemistry ,Fluorescence ,Fluorescence spectroscopy ,0104 chemical sciences ,Analytical Chemistry ,Transmission electron microscopy ,Quantum dot ,Nanorod ,Inductively coupled plasma ,0210 nano-technology ,High-resolution transmission electron microscopy - Abstract
This work established a fluorescence approach for detecting ascorbic acid (AA) based on Cu-ZnCdS quantum dots (Cu-ZnCdS QDs) and α-MnO2 nanorods. Cu-ZnCdS QDs and α-MnO2 nanorods were characterized by high-resolution transmission electron microscopy (HRTEM), fluorescence spectroscopy, inductively coupled plasma optical emission spectroscopy (ICP-OES) and X-ray diffraction (XRD). In the presence of α-MnO2 nanorods, the fluorescence of Cu-ZnCdS QDs was greatly quenched through the inner filter effect (IFE). Subsequently, AA can trigger the decomposition of the α-MnO2 nanorods which can reduce α-MnO2 to Mn2+ and recover the fluorescence. Under optimal conditions, a linear relation was obtained over the range 5.02-401.77 μM with a 31.62 μM detection limit. Through applying the fluorescent sensing system for detecting AA, a satisfactory result is obtained with recoveries ranging from 89.23% to 110.99%.
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- 2017
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19. Modeling plasmas in analytical chemistry-an example of cross-fertilization
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Annemie Bogaerts
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Glow discharge ,Laser ablation ,Materials science ,Atmospheric pressure ,010401 analytical chemistry ,Analytical chemistry ,02 engineering and technology ,Plasma ,021001 nanoscience & nanotechnology ,01 natural sciences ,Biochemistry ,0104 chemical sciences ,Analytical Chemistry ,Spectrochemistry ,Chemistry ,Ionization ,Inductively coupled plasma ,0210 nano-technology ,Spectroscopy ,Biology - Abstract
This paper gives an overview of the modeling work developed in our group in the last 25 years for various plasmas used in analytical spectrochemistry, i.e., glow discharges (GDs), inductively coupled plasmas (ICPs), and laser ablation (LA) for sample introduction in the ICP and for laser-induced breakdown spectroscopy (LIBS). The modeling approaches are briefly presented, which are different for each case, and some characteristic results are illustrated. These plasmas are used not only in analytical chemistry but also in other applications, and the insights obtained in these other fields were quite helpful for us to develop models for the analytical plasmas. Likewise, there is now a huge interest in plasma-liquid interaction, atmospheric pressure glow discharges (APGDs), and dielectric barrier discharges (DBDs) for environmental, medical, and materials applications of plasmas. The insights obtained in these fields are also very relevant for ambient desorption/ionization sources and for liquid sampling, which are nowadays very popular in analytical chemistry, and they could be very helpful in developing models for these sources as well. Graphical abstract.
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- 2019
20. Determination of the isotopic composition of lutetium using MC-ICPMS
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Xiandeng Hou, Chengbin Zheng, Zoltán Mester, Juan He, Juris Meija, and Lu Yang
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Materials science ,Analytical chemistry ,chemistry.chemical_element ,02 engineering and technology ,Fractionation ,isotopic fractionation/mass bias ,01 natural sciences ,Biochemistry ,isotopic abundances ,Analytical Chemistry ,regression model ,Isotope ,010401 analytical chemistry ,Rhenium ,021001 nanoscience & nanotechnology ,Lutetium ,Atomic mass ,0104 chemical sciences ,chemistry ,atomic weight ,MC-ICPMS ,Primary standard ,Measurement uncertainty ,isotope ratio ,Inductively coupled plasma ,0210 nano-technology - Abstract
In this study, we report the first independent measurements of lutetium isotopic composition using multi-collector ICPMS in four commercial lutetium materials, including a new NRC candidate lutetium isotopic reference material, LUIS-1. The regression model was used to correct for the instrumental isotopic fractionation (mass bias) using NIST SRM 989 isotopic rhenium as the primary calibrator. The regression model is based on a short 15-min measurement sessions at varying ICP plasma power. Isotope ratio of R176/175 = 0.026553(11)k = 1, corresponding isotopic abundances of x176 = 0.025866(11)k = 1, x175 = 0.974134(11)k = 1, and an atomic weight of Ar(Lu) = 174.966693(13)k = 1 were obtained for lutetium in LUIS-1. Uncertainty estimation was performed using a mixture of modeling approaches in accordance with the JCGM 100:2008 “Guide to the Expression of Uncertainty in Measurement” and its Supplement 1. The relative contribution of the rhenium primary standard to the combined uncertainty of 176Lu/175Lu isotope ratio was 15%.
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- 2019
21. Investigation of various layered lithium ion battery cathode materials by plasma- and X-ray-based element analytical techniques
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Marco Evertz, Martin Winter, Sascha Nowak, and Johannes Kasnatscheew
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Materials science ,010401 analytical chemistry ,Analytical chemistry ,chemistry.chemical_element ,02 engineering and technology ,Electrolyte ,021001 nanoscience & nanotechnology ,01 natural sciences ,Biochemistry ,Lithium-ion battery ,Cathode ,0104 chemical sciences ,Analytical Chemistry ,Anode ,law.invention ,Nickel ,chemistry ,law ,Inductively coupled plasma ,0210 nano-technology ,Capacity loss ,Separator (electricity) - Abstract
In this work, the transition metal dissolution (TMD) from the respective ternary layered LiMO2 (M = Mn, Co, Ni, Al) cathode active material was investigated as well as the lithiation degrees of the cathodes after charge/discharge cyclic aging. Furthermore, increased nickel contents in LiNixCoyMnzO2-based (NCM) cathode materials were studied, to elucidate their influence on capacity fading and TMD. It was found, that the TMD from nickel-rich cathode materials, e.g., LiNi0.6Co0.2Mn0.2O2 or LiNi0.8Co0.1Mn0.1O2, did not differ significantly from the TMD from the stoichiometric LiNi1/3Co1/3Mn1/3O2. In detail, the TMD from the cathode did not exceed a maximum of 0.2 wt% and was uniformly distributed on all analyzed cell parts (separator, anode, and electrolyte) using total reflection X-ray fluorescence. Moreover, the investigated electrolyte solutions showed that increased Ni contents come with more nickel dissolution of the respective material. Additionally, inductively coupled plasma optical emission spectroscopy analysis on the respective charge/discharge cyclic-aged cathode active materials revealed lithium losses of 20% after 50 cycles. However, only a minimum amount of capacity loss (= 1.5 mAh g−1) can be attributed to active material loss.
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- 2018
22. A combined chemical imaging approach using (MC) LA-ICP-MS and NIR-HSI to evaluate the diagenetic status of bone material for Sr isotope analysis
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Jörg Feldmann, Maria Teschler-Nicola, Johanna Irrgeher, Magdalena Blanz, Thomas Prohaska, Anika Retzmann, and Andreas Zitek
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Chemical imaging ,Analytical chemistry ,02 engineering and technology ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Bone and Bones ,Mass Spectrometry ,Analytical Chemistry ,Strontium Isotopes ,Animals ,Humans ,Solubility ,Humic Substances ,Isotope analysis ,Laser ablation ,Spectroscopy, Near-Infrared ,Isotope ,Chemistry ,Lasers ,010401 analytical chemistry ,Reproducibility of Results ,021001 nanoscience & nanotechnology ,Isotopes of strontium ,0104 chemical sciences ,Molecular Imaging ,Inductively coupled plasma ,0210 nano-technology - Abstract
This paper presents a combination of elemental and isotopic spatial distribution imaging with near-infrared hyperspectral imaging (NIR-HSI) to evaluate the diagenetic status of skeletal remains. The aim is to assess how areas with biogenic n(87Sr)/n(86Sr) isotope-amount ratios may be identified in bone material, an important recorder complementary to teeth. Elemental (C, P, Ca, Sr) and isotopic (n(87Sr)/n(86Sr)) imaging were accomplished via laser ablation (LA) coupled in a split stream to a quadrupole inductively coupled plasma mass spectrometer (ICP-QMS) and a multicollector inductively coupled plasma mass spectrometer (MC ICP-MS) (abbreviation for the combined method LASS ICP-QMS/MC ICP-MS). Biogenic areas on the bone cross section, which remained unaltered by diagenetic processes, were localized using chemical indicators (I(C)/I(Ca) and I(C) × 10/I(P) intensity ratios) and NIR-HSI at a wavelength of 1410 nm to identify preserved collagen. The n(87Sr)/n(86Sr) isotope signature analyzed in these areas was in agreement with the biogenic bulk signal revealed by solubility profiling used as an independent method for validation. Elevated C intensities in the outer rim of the bone, caused by either precipitated secondary minerals or adsorbed humic materials, could be identified as indication for diagenetic alteration. These areas also show a different n(87Sr)/n(86Sr) isotopic composition. Therefore, the combination of NIR-HSI and LASS ICP-QMS/MC ICP-MS allows for the determination of preserved biogenic n(87Sr)/n(86Sr) isotope-amount ratios, if the original biogenic material has not been entirely replaced by diagenetic material.
- Published
- 2018
23. Development of certified reference materials for electrolytes in human serum (GBW09124-09126)
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Jun Wang, Yanjie Cui, Liuxing Feng, Hongmei Li, Haifeng Li, and Naijie Shi
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Serum ,Ion chromatography ,Analytical chemistry ,Magnesium Chloride ,Electrolyte ,Isotope dilution ,010502 geochemistry & geophysics ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,law.invention ,Potassium Chloride ,Electrolytes ,Lithium Carbonate ,law ,Humans ,Inductively coupled plasma mass spectrometry ,0105 earth and related environmental sciences ,Radioisotopes ,Chemistry ,010401 analytical chemistry ,Oxides ,Calcium Compounds ,0104 chemical sciences ,Certified reference materials ,Inductively coupled plasma ,Atomic absorption spectroscopy ,Mass fraction ,Blood Chemical Analysis - Abstract
Three reference materials, at relatively low, middle, and high concentrations, were developed for analysis of the mass fractions of electrolytes (K, Ca, Na, Mg, Cl, and Li) in human serum. The reference materials were prepared by adding high purity chloride salts to normal human serum. The concentration range of the three levels is within ±20% of normal human serum. It was shown that 14 units with duplicate analysis is enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for 1 week at 40 °C and long-term stability test for 14 months. The certification methods of the six elements include isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectroscopy (ICP-OES), atomic absorption spectroscopy (AAS), ion chromatography (IC), and ion-selective electrode (ISE). The certification methods were validated by international comparisons among a number of national metrology institutes (NMIs). The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the analytical methods, homogeneity, and stability. The range of the expanded uncertainties of all the elements is from 2.2% to 3.9%. The certified reference materials (CRMs) are primarily intended for use in the calibration and validation of procedures in clinical analysis for the determination of electrolytes in human serum or plasma. Graphical Abstract Certified reference materials for K, Ca, Mg, Na, Cl and Li in human serum (GBW09124-09126).
- Published
- 2017
24. Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium
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Carola Pape, Heinrich Kipphardt, Volker Görlitz, Silke Richter, Angela Kaltenbach, Bernd Güttler, Gernot Kopp, Reinhard Jährling, Janine Noordmann, and Olaf Rienitz
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Chemistry ,Molybdenum ,Inductively coupled plasma atomic emission spectroscopy ,Calibration ,Analytical chemistry ,Gravimetric analysis ,chemistry.chemical_element ,Inductively coupled plasma ,Biochemistry ,Inductively coupled plasma mass spectrometry ,Mass fraction ,Analytical Chemistry ,Metrology - Abstract
Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.
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- 2014
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25. Recognizing and overcoming analytical error in the use of ICP-MS for the determination of cadmium in breakfast cereal and dietary supplements
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Karen E. Murphy and Thomas W. Vetter
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Analytical chemistry ,Indicator Dilution Techniques ,chemistry.chemical_element ,Isotope dilution ,Mass spectrometry ,Biochemistry ,Analytical Chemistry ,Isotopes ,Reference Values ,Spectrophotometry ,medicine ,Humans ,Inductively coupled plasma mass spectrometry ,Cadmium ,Chromatography ,medicine.diagnostic_test ,Isotope ,Spectrophotometry, Atomic ,Reproducibility of Results ,Vitamins ,Reference Standards ,chemistry ,Dietary Supplements ,Food, Fortified ,Inductively coupled plasma ,Artifacts ,Edible Grain ,Multivitamin - Abstract
The potential effect of spectral interference on the accurate measurement of the cadmium (Cd) mass fraction in fortified breakfast cereal and a variety of dietary supplement materials using inductively coupled plasma quadrupole mass spectrometry was studied. The materials were two new standard reference materials (SRMs)--SRM 3233 Fortified Breakfast Cereal and SRM 3532 Calcium Dietary Supplement--as well as several existing materials--SRM 3258 Bitter Orange Fruit, SRM 3259 Bitter Orange Extract, SRM 3260 Bitter Orange-containing Solid Oral Dosage Form, and SRM 3280 Multivitamin/Multielement Tablets. Samples were prepared for analysis using the method of isotope dilution and measured using various operating and sample introduction configurations including standard mode, collision cell with kinetic energy discrimination mode, and standard mode with sample introduction via a desolvating nebulizer system. Three isotope pairs, (112)Cd/(111)Cd, (113)Cd/(111)Cd, and (114)Cd/(111)Cd, were measured. Cadmium mass fraction results for the unseparated samples of each material, measured using the three instrument configurations and isotope pairs, were compared to the results obtained after the matrix was removed via chemical separation using anion exchange chromatography. In four of the six materials studied, measurements using the standard mode with sample introduction via the desolvating nebulizer gave results for the unseparated samples quantified with the (112)Cd/(111)Cd isotope pair that showed a positive bias relative to the matrix-separated samples, which indicated a persistent inference at m/z112 with this configuration. Use of the standard mode, without the desolvating nebulizer, also gave results that showed a positive bias for the unseparated samples quantified with the (112)Cd/(111)Cd isotope pair in three of the materials studied. Collision cell/kinetic energy discrimination mode, however, was very effective for reducing spectral interference for Cd in all of the materials and isotope pairs studied, except in the multivitamin/multielement matrix (SRM 3280) where the large corrections for known isobaric interferences or unidentified interferences compromised the accuracy. For SRM 3280, matrix separation provided the best method to achieve accurate measurement of Cd.
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- 2013
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26. On-line dynamic extraction system hyphenated to inductively coupled plasma optical emission spectrometry for automatic determination of oral bioaccessible trace metal fractions in airborne particulate matter
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Manuel Miró, Victoria Mohr, and Andreas Limbeck
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Analyte ,Analytical chemistry ,010501 environmental sciences ,01 natural sciences ,Biochemistry ,Online Systems ,Mass Spectrometry ,Analytical Chemistry ,Metal ,Humans ,Trace metal ,Optical emission spectrometry ,0105 earth and related environmental sciences ,Chromatography ,Gastric Juice ,Gastric fluid ,Chemistry ,010401 analytical chemistry ,Particulates ,0104 chemical sciences ,Trace Elements ,Metals ,visual_art ,visual_art.visual_art_medium ,Particulate Matter ,Leaching (metallurgy) ,Inductively coupled plasma ,Environmental Monitoring - Abstract
For a realistic evaluation of the potential hazard emanating from airborne particulate matter (APM), the determination of the total inhaled metal amounts associated with APM is insufficient in risk assessment. Additional information about metal fractions that can be mobilized by the human body is necessary, because only those soluble (also called bioaccessible) fractions can be absorbed by the human body, and thus potentially cause adverse health effects. In the present study, a dynamic flow-through approach as a front end to inductively coupled plasma optical emission spectrometry (ICP-OES) exploiting advanced flow analysis is employed for on-line handling of multiple APM samples and determination of bioaccessible trace metals under worst case extraction scenarios. The method is based on on-line continuous extraction of filter samples with synthetic gastric fluid followed by on-line ICP-OES measurement of the dissolved fraction of trace metals. The assembly permits an automated successive measurement of three sample replicates in less than 19 min. The on-line extraction procedure offers increased sample throughput and reduced risk of sample contamination and overcomes metal re-adsorption processes compared to the traditional batch-wise counterparts. Furthermore, it provides deeper information on the kinetics of the leaching process. The developed procedure was applied to the determination of bioaccessible metal fractions (Al, Ba, Cu, Fe and Mn as model analytes) in PM10 samples from Palma de Mallorca (Spain) and Vienna (Austria). Graphical Abstract On-line gastric bioaccessibility of elements in airborne particulate matter.
- Published
- 2016
27. A matrix effect and accuracy evaluation for the determination of elements in milk powder LIBS and laser ablation/ICP-OES spectrometry
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Qianli Ma, N. Gilon, Jin Yu, Wenqi Lei, A. Stankova, J. El-Haddad, Vincent Motto-Ros, ANALISS - Analyse inorganique, spectroscopie et spéciation (2011-2013), Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Spectrométrie Ionique et Moléculaire (LASIM), and Université Claude Bernard Lyon 1 (UCBL)
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Analytical chemistry ,MESH: Spectrum Analysis ,02 engineering and technology ,DIAGNOSTICS ,MESH: Powders ,MESH: Zinc ,01 natural sciences ,Biochemistry ,SOLUTION NEBULIZATION ,Analytical Chemistry ,law.invention ,law ,Spectrophotometry ,MESH: Magnesium ,WATER ,MESH: Sodium ,Magnesium ,MESH: Animals ,Laser-induced plasma ,MESH: Spectrophotometry, Atomic ,TEMPERATURE ,Temperatures ,Laser ablation ,medicine.diagnostic_test ,Chemistry ,Rotational temperature ,021001 nanoscience & nanotechnology ,MESH: Temperature ,Zinc ,Milk ,MESH: Calcium ,Inductively coupled plasma atomic emission spectroscopy ,Calibration ,MESH: Lasers ,Female ,Powders ,Inductively coupled plasma ,0210 nano-technology ,Matrix effects ,Mass spectrometry ,Sensitivity and Specificity ,Optical spectrometry ,MESH: Calibration ,INDUCTIVELY-COUPLED PLASMA ,[CHIM.ANAL]Chemical Sciences/Analytical chemistry ,EXCITATION ,medicine ,Animals ,[SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM] ,Spectroscopy ,Lasers ,Spectrophotometry, Atomic ,Spectrum Analysis ,Sodium ,010401 analytical chemistry ,Laser ,MESH: Sensitivity and Specificity ,0104 chemical sciences ,MESH: Milk ,Calcium ,EMISSION ,MESH: Female - Abstract
International audience; Laser ablation coupled to inductively coupled plasma optical emission spectrometry (LA-ICP-OES) and laser-induced breakdown spectroscopy (LIBS) were investigated for the determination of Ca, Mg, Zn and Na in milk samples. The accuracy of both methods was evaluated by comparison of the concentration found using LA-ICP-OES and LIBS with classical wet digestion associated with ICP-OES determination. The results were not fully acceptable, with biases from less than 1% to more than 60%. Matrix effects were also investigated. The sample matrix can influence the temperature, electron number density (n (e)) and other excitation characteristics in the ICP. These ICP characteristics were studied and evaluated during ablation of eight milk samples. Differences in n (e) (from 8.9 to 13.8 × 10(14) cm(-3)) and rotational temperature (ranging from 3,400 to 4,400 K) occurred with no correlation with trueness. LIBS results obtained after classical external calibration procedure gave degraded accuracy, indicating a strong matrix effect. The LIBS measurements clearly showed that the major problem in LA-ICP was related to the ablation process and that LIBS spectroscopy is an excellent diagnostic tool for LA-ICP techniques.
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- 2011
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28. Quantitative analysis of slurry sample by laser-induced breakdown spectroscopy
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Fang-Yu Yueh, Laura T. Smith, Jagdish P. Singh, Krishna K. Ayyalasomayajula, and Vivek Dikshit
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Chemistry ,Linear regression ,Partial least squares regression ,Slurry ,Calibration ,Analytical chemistry ,Laser-induced breakdown spectroscopy ,Inductively coupled plasma ,Spectroscopy ,Biochemistry ,Quantitative analysis (chemistry) ,Analytical Chemistry - Abstract
Laser-induced breakdown spectroscopy (LIBS) has been employed for the analysis of slurry samples. Quantitative analysis of slurry samples is crucial and challenging. The problems associated with slurry samples include splashing, surface turbulence, and the difficulties of obtaining reproducible samples due to sedimentation. The LIBS analysis has achieved limited success due to inherent disadvantages when applied to slurry samples. In order to achieve improved measurement precision and accuracy, a spin-on-glass sampling method was evaluated. Five elements (Al, Ca, Fe, Ni, and Si) were examined in five slurry simulants containing varying amounts of each ion. Three calibration models were developed by using univariate calibration, multiple linear regression, and partial least square regression. LIBS analysis results obtained from the partial least square regression model were determined to be the best fit to results obtained from inductively coupled plasma optical emission spectroscopy analysis.
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- 2011
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29. Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy
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A. Stankova, Wenqi Lei, H. P. Zeng, J. El Haddad, Vincent Motto-Ros, Qianli Ma, L. J. Zheng, Jin Yu, N. Gilon-Delepine, Xueshi Bai, Laboratoire de Spectrométrie Ionique et Moléculaire (LASIM), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), State Key Lab Precis Spect, East China Normal University [Shangaï] (ECNU), Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), ANALISS - Analyse inorganique, spectroscopie et spéciation (2011-2013), and Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL)
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Milk powder ,SAMPLES ,ALLOYS ,Analytical chemistry ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Analytical Chemistry ,010309 optics ,[CHIM.ANAL]Chemical Sciences/Analytical chemistry ,0103 physical sciences ,TRACE-ELEMENTS ,Methods ,Calibration ,Animals ,Laser-induced breakdown spectroscopy ,[SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM] ,SELF-ABSORPTION ,Spectroscopy ,Matrix effect ,Minerals ,LIBS ,Laser ablation ,Chemistry ,ICP-AES ,AIR ,Spectrum Analysis ,010401 analytical chemistry ,Plasma ,CF-LIBS ,QUANTITATIVE-ANALYSIS ,Elements ,SOILS ,0104 chemical sciences ,Milk ,SPECTROMETRY ,Metals ,Inductively coupled plasma atomic emission spectroscopy ,Powders ,Inductively coupled plasma ,Food Analysis - Abstract
International audience; Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials
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- 2011
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30. Nondestructive analysis of single crystals of selenide spinels by X-ray spectrometry techniques
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Beata Zawisza, J. Heimann, Andrzej Kita, Rafal Sitko, Dariusz Kajewski, and Ewa Malicka
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Original Paper ,Chemistry ,Analytical chemistry ,Fluorescence spectrometry ,Mass spectrometry ,Biochemistry ,Chalcogenide compounds ,Analytical Chemistry ,chemistry.chemical_compound ,X-ray photoelectron spectroscopy ,Elemental analysis ,Sputtering ,Selenide ,Nondestructive analysis ,XPS ,Sample preparation ,EPMA ,Inductively coupled plasma ,Micro-XRF ,Selenide spinel - Abstract
The paper presents possibilities and difficulties in nondestructive analysis of small multielement single crystals performed by means of X-ray spectrometry techniques: micro-X-ray fluorescence spectrometry (μ-XRF), energy-dispersive electron probe microanalysis (ED-EPMA), and X-ray photoelectron spectroscopy (XPS). The capability of the X-ray spectroscopy techniques in elemental analysis is demonstrated with the single crystals of selenide spinels of the general formula MxNyCrzSe4 (M+2 and N+3 are, for example, Zn+2, V+3, Ga+3, Cd+2, In+3, and Sb+3). The results of the nondestructive analyses (μ-XRF, ED-EPMA, and XPS) are compared with those obtained by inductively coupled plasma optical emission spectrometry (ICP-OES) and wavelength-dispersive X-ray spectrometry (WDXRF) following sample digestion. The present study shows satisfactory agreement between the results of μ-XRF analysis performed using the standardless fundamental parameter method and the results obtained with the WDXRF and ICP-OES analyses. If the measured single crystal is precisely positioned, the difference between μ-XRF and wet analysis (WDXRF and ICP-OES) does not exceed 5% rel. The reliable results of ED-EPMA can be obtained only if the measured area is sufficiently large, i.e., of 200 × 300 μm. Even if this condition is fulfilled, the relative difference between the ED-EPMA and the wet analysis may reach 10% rel. In case of the XPS analysis, the accuracy of results depends on the proper preparation of the sample surface. It should be free of contamination that can be obtained by scraping in situ in ultrahigh vacuum. The ion etching, commonly used for cleaning the surface, leads to preferential sputtering; therefore, the reliable results cannot be obtained. Figure The paper presents possibilities and difficulties in nondestructive analysis of small multielement single crystals performed by means of X-ray spectrometry techniques: micro-XRF, ED-EPMA and XPS.
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- 2010
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31. Spectroscopic and analytical characteristics of an inductively coupled argon plasma combined with hydride generation with or without simultaneous introduction of the sample aerosol for optical emission spectrometry
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Pawel Pohl and José A. C. Broekaert
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Detection limit ,Argon ,Chemistry ,Hydride ,Analytical chemistry ,chemistry.chemical_element ,Excitation temperature ,Plasma ,Biochemistry ,Analytical Chemistry ,Metal ,visual_art ,Ionization ,visual_art.visual_art_medium ,Inductively coupled plasma - Abstract
A radially viewed inductively coupled argon plasma was used for optical emission spectrometry of volatile species formed by reaction with NaBH(4) (hydride generation). The volatile hydrides were either introduced into the plasma alone or at the same time as a sample aerosol generated by pneumatic nebulization with a commercially available Concomitant Metals Analyzer. The effects of the forward power, the presence of pre-reducing agents [(NH(2))(2)SC, KI, KBr and hot HCl], the occurrence of easily ionized elements (Ca, K, Mg and Na) in the analyte solutions on the excitation temperature (as measured via Ar atomic lines) and the electron number density were investigated for both of the sample introduction modes applied. The detection limits and the signal-to-background intensity ratios for As, Bi, Sb, Se and Sn lines were also evaluated and were observed to deteriorate with increasing power. When simultaneous hydride generation and pneumatic nebulization was employed under optimized experimental conditions, detection limits of 3.5, 2.9, 4.3, 1.5 and 2.1 microg L(-1) for As, Bi, Sb, Se and Sn, respectively, were obtained, and the intensities of the analytical lines for elements that do not form volatile hydrides were found to be 40% (Cd), 30% (Ni), 20% (Co, Cr, Fe, Mn and Zn) and 10% (Cu, Mg, V) greater than those obtained when only pneumatic nebulization was used.
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- 2010
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32. Ionomic profiling of Nicotiana langsdorffii wild-type and mutant genotypes exposed to abiotic stresses
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Ardini, Francisco, Soggia, Francesco, Abelmoschi, Maria Luisa, Magi, Emanuele, and Grotti, Marco
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- 2013
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33. On-line ionic imprinted polymer selective solid-phase extraction of nickel and lead from seawater and their determination by inductively coupled plasma-optical emission spectrometry
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Natalia García-Otero, Carmen Teijeiro-Valiño, Elena Peña-Vázquez, Pilar Bermejo-Barrera, Antonio Moreda-Piñeiro, and Jacobo Otero-Romaní
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Detection limit ,Nickel ,Certified reference materials ,chemistry ,Elution ,Analytical chemistry ,Precipitation polymerization ,chemistry.chemical_element ,Solid phase extraction ,Inductively coupled plasma ,Enrichment factor ,Biochemistry ,Analytical Chemistry - Abstract
Nickel(II) and lead(II) ionic imprinted 8-hydroxyquinoline polymers were synthesized by a precipitation polymerization technique and were used as selective solid phase extraction supports for the determination of nickel and lead in seawater by flow injection solid phase extraction on-line inductively coupled plasma-optical emission spectrometry. An optimum loading flow rate of 2.25 mL min(-1) for 2 min and an elution flow rate of 2.25 mL min(-1) for 1 min gave an enrichment factor of 15 for nickel. However, a low dynamic capacity and/or rate for adsorption and desorption was found for lead ionic imprinted polymer and a flow rate of 3.00 mL min(-1) for 4-min loading and a flow rate of 2.25 mL min(-1) for 1-min elution gave a enrichment factor of 5. The limit of detection was 0.33 microg L(-1) for nickel and 1.88 microg L(-1) for lead, with a precision (n = 11) of 8% (2.37 microg Ni L(-1)) for nickel and 11% (8.38 microg Pb L(-1)) for lead. Accuracy was also assessed by analyzing SLEW-3 (estuarine water) and TM-24 (lake water) certified reference materials, and the values determined were in good agreement with the certified concentrations.
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- 2009
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34. Determination of glyphosate and AMPA in surface and waste water using high-performance ion chromatography coupled to inductively coupled plasma dynamic reaction cell mass spectrometry (HPIC–ICP–DRC–MS)
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Gerhard Stingeder, Axel Mentler, Stephan Hann, Maximilian Popp, Gunda Koellensperger, and Maria Fuerhacker
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Spectrometry, Mass, Electrospray Ionization ,Chromatography ,Ion exchange ,Chemistry ,Electrospray ionization ,Ion chromatography ,Glycine ,Organophosphonates ,Pesticide Residues ,Tetrazoles ,Water ,Isoxazoles ,Chromatography, Ion Exchange ,Mass spectrometry ,Waste Disposal, Fluid ,Biochemistry ,Analytical Chemistry ,Chelex 100 ,chemistry.chemical_compound ,Inductively coupled plasma ,Inductively coupled plasma mass spectrometry ,Chromatography, High Pressure Liquid ,Water Pollutants, Chemical ,Waste disposal - Abstract
A novel method employing high-performance cation chromatography in combination with inductively coupled plasma dynamic reaction cell mass spectrometry (ICP-DRC-MS) for the simultaneous determination of the herbicide glyphosate (N-phosphonomethylglycine) and its main metabolite aminomethyl phosphonic acid (AMPA) is presented. P was measured as (31)P(16)O(+) using oxygen as reaction gas. For monitoring the stringent target value of 0.1 μg L(-1) for glyphosate, applicable for drinking and surface water within the EU, a two-step enrichment procedure employing Chelex 100 and AG1-X8 resins was applied prior to HPIC-ICP-MS analysis. The presented approach was validated for surface water, revealing concentrations of 0.67 μg L(-1) glyphosate and 2.8 μg L(-1) AMPA in selected Austrian river water samples. Moreover, investigations at three waste water-treatment plants showed that elimination of the compounds at the present concentration levels was not straightforward. On the contrary, all investigated plant effluents showed significant amounts of both compounds. Concentration levels ranged from 0.5-2 μg L(-1) and 4-14 μg L(-1) for glyphosate and AMPA, respectively.
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- 2008
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35. μLC coupled to ICP–SFMS with post-column isotope dilution analysis of sulfur for absolute protein quantification
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Ralf Krüger, Jörg Bettmer, Nico Zinn, and Peter Leonhard
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Radioisotope Dilution Technique ,Spectrometry, Mass, Electrospray Ionization ,Bioanalysis ,Chromatography ,Apolipoprotein A-I ,Elution ,Chemistry ,Analytical chemistry ,Proteins ,Isotope dilution ,Mass spectrometry ,Biochemistry ,Analytical Chemistry ,Certified reference materials ,Limit of Detection ,Sulfur Isotopes ,Animals ,Humans ,Amino Acid Sequence ,alpha-Fetoproteins ,Inductively coupled plasma ,Quantitative analysis (chemistry) ,Inductively coupled plasma mass spectrometry ,Chromatography, High Pressure Liquid - Abstract
Absolute protein quantification has become an important challenge in modern bioanalytical chemistry. Among several approaches based on mass spectrometric techniques, inductively coupled plasma (ICP) as ionisation source provides element-selective and sensitive detection of heteroatoms, and thus, a potentially emerging tool in protein analysis. In this work we applied coupling of capillary liquid chromatography (μLC) and inductively coupled plasma-sector field mass spectrometry (ICP-SFMS) to the separation and determination of standard proteins. For quantification purposes, post-column isotope dilution of sulfur was applied and optimised for this type of hyphenated technique. Provided that the protein sequence is known (number of sulfur-containing amino acids, i.e. cysteines and methionines) the protein amount can then be directly calculated from the determined sulfur content in a certain protein fraction. In order to prove the reliability of the presented method, two different certified reference materials were analysed: CRM 393 (human apolipoprotein A-I) and CRM 486 (α-fetoprotein). For CRM 393 excellent agreement (37.0 ± 1.4 μmol L(-1)) was obtained with the certificate (37.7 ± 1.8 μmol L(-1)). However, the recovery rate for α-fetoprotein in CRM 486 was found to be about 60% indicating incomplete elution of the protein during the chromatographic separation.
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- 2008
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36. Synthesis of chitosan resin possessing a phenylarsonic acid moiety for collection/concentration of uranium and its determination by ICP-AES
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Kenji Seo, Koji Oshita, Akhmad Sabarudin, Shoji Motomizu, Toshio Takayanagi, and Mitsuko Oshima
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Time Factors ,chemistry.chemical_element ,Mass spectrometry ,Sensitivity and Specificity ,Biochemistry ,Arsenicals ,Analytical Chemistry ,chemistry.chemical_compound ,Adsorption ,Nitric acid ,Detection limit ,Chitosan ,Chromatography ,Molecular Structure ,Spectrophotometry, Atomic ,technology, industry, and agriculture ,Reproducibility of Results ,Phenylarsonic acid ,Uranium ,Resins, Synthetic ,chemistry ,Inductively coupled plasma atomic emission spectroscopy ,Inductively coupled plasma ,Nuclear chemistry - Abstract
A chitosan resin possessing a phenylarsonic acid moiety (phenylarsonic acid type chitosan resin) was developed for the collection and concentration of trace uranium prior to inductively coupled plasma (ICP) atomic emission spectrometry (AES) measurement. The adsorption behavior of 52 elements was systematically examined by packing it in a minicolumn and measuring the elements in the effluent by ICP mass spectrometry. The resin could adsorb several cationic species by a chelating mechanism, and several oxo acids, such as Ti(IV), V(V), Mo(VI), and W(VI), by an anion-exchange mechanism and/or a chelating mechanism. Especially, U(VI) could be adsorbed almost 100% over a wide pH region from pH 4 to 8. Uranium adsorbed was easily eluted with 1 M nitric acid (10 mL), and the 25-fold preconcentration of uranium was achieved by using a proposed column procedure, which could be applied to the determination of trace uranium in seawater by ICP-AES. The limit of detection was 0.1 ng mL(-1) for measurement by ICP-AES coupled with 25-fold column preconcentration.
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- 2008
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37. Improving detection power in trace analysis using wavelet transform
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Prikler, Simon and Einax, Jürgen W.
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- 2012
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38. Complementary molecular and elemental detection of speciated thioarsenicals using ESI-MS in combination with a xenon-based collision-cell ICP-MS with application to fortified NIST freeze-dried urine
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John T. Creed, Patricia A. Creed, Christina M. Gallawa, Jenny L. Ellis, Joseph A. Caruso, Kevin M. Kubachka, Andrea R. Young, and Sean D. Conklin
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Spectrometry, Mass, Electrospray Ionization ,Xenon ,Electrospray ionization ,Analytical chemistry ,chemistry.chemical_element ,Urine ,Mass spectrometry ,Sensitivity and Specificity ,Biochemistry ,Arsenicals ,Mass Spectrometry ,Arsenic ,Analytical Chemistry ,chemistry.chemical_compound ,Inductively coupled plasma mass spectrometry ,Chromatography, High Pressure Liquid ,Detection limit ,Chemical ionization ,Chromatography ,Chemistry ,Reproducibility of Results ,Arsenamide ,Trimethylarsine ,Freeze Drying ,Inductively coupled plasma ,Sulfur - Abstract
The simultaneous detection of arsenic and sulfur in thioarsenicals was achieved using xenon-based collision-cell inductively coupled plasma (ICP) mass spectrometry (MS) in combination with high-performance liquid chromatography. In an attempt to minimize the (16)O(16)O(+) interference at m/z 32, both sample introduction and collision-cell experimental parameters were optimized. Low flow rates (0.25 mL/min) and a high methanol concentration (8%) in the mobile phase produced a fourfold decrease in the m/z 32 background. A plasma sampling depth change from 3 to 7 mm produced a twofold decrease in background at m/z 32, with a corresponding fourfold increase in the signal associated with a high ionization surrogate for sulfur. The quadrupole bias and the octopole bias were used as a kinetic energy discriminator between background and analyte ions, but a variety of tuning conditions produced similar (less than twofold change) detection limits for sulfur ((32)S). A 34-fold improvement in the (32)S detection limit was achieved using xenon instead of helium as a collision gas. The optimized xenon-based collision cell ICP mass spectrometer was then used with electrospray ionization MS to provide elemental and molecular-based information for the analysis of a fortified sample of NIST freeze-dried urine. The 3sigma detection limits, based on peak height for dimethylthioarsinic acid (DMTA) and trimethylarsine sulfide (TMAS), were 15 and 12 ng/g, respectively. Finally, the peak area reproducibilities (percentage relative standard deviation) of a 5-ppm fortified sample of NIST freeze dried urine for DMTA and TMAS were 7.4 and 5.4%, respectively.
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- 2007
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39. Determination of impurities in magnesium niobate by slurry introduction axially viewed inductively coupled plasma optical emission spectrometry
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Pingang He, Anbao Wang, Yuzhi Fang, Haiyun Qu, Dongmei Wu, and Min Dong
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Sodium polyacrylate ,Calibration curve ,Magnesium ,Analytical chemistry ,chemistry.chemical_element ,Biochemistry ,Dispersant ,Analytical Chemistry ,chemistry.chemical_compound ,chemistry ,Slurry ,Particle size ,Inductively coupled plasma ,Dispersion (chemistry) - Abstract
A simple preparation scheme is described for the quantitative analysis of a magnesium niobate sample using slurry introduction axially viewed inductively coupled plasma optical emission spectrometry. Relationships between the stability of slurries and the conditions, such as particle size, pH, dispersant and amount of dispersant, were investigated experimentally. The MgNb(2)O(6) slurry sample was prepared by adding the dispersant sodium polyacrylate and agitation in an ultrasonic bath to ensure good dispersion. Under optimization of pH and amount of dispersant, an analysis of minor and trace impurities (Ba, Ca, Cr, Cu, Fe, Mn, Ni, Pb) in magnesium niobate was accomplished. Applying a paired t test, we showed that the results were in agreement at a 95% confidence level with the reference values obtained by a fusion method for a magnesium niobate sample, which verified that the calibration curves could be established by aqueous standards. Analytical results demonstrate that the factors that affected the accuracy of determination for MgNb(2)O(6) are mainly the particle size of the sample and the stability of slurry.
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- 2007
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40. Ultratrace-level radium-226 determination in seawater samples by isotope dilution inductively coupled plasma mass spectrometry
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Zsolt Varga
- Subjects
Detection limit ,Chromatography ,Resolution (mass spectrometry) ,Environmental analysis ,Chemistry ,Sample preparation ,Isotope dilution ,Inductively coupled plasma ,Mass spectrometry ,Biochemistry ,Inductively coupled plasma mass spectrometry ,Analytical Chemistry - Abstract
An improved and novel sample preparation method for 226Ra determination in liquid samples by isotope dilution inductively coupled plasma sector field mass spectrometry using laboratory-prepared 228Ra tracer has been developed. The procedure involves a selective preconcentration achieved by applying laboratory-prepared MnO2 resin followed by cation exchange chromatographic separation. In order to completely eliminate possible molecular interferences, medium mass resolution (R = 4,000) combined with chemical separation was found to be a good compromise that enhanced the reliability of the method. The detection limit of 0.084 fg g(-1) (3.1 mBq kg(-1)) achieved is comparable to that of the emanation method or alpha spectrometry and is suitable for low-level environmental measurements. The chemical recovery of the sample preparation method ranged from 72 to 94%. The proposed method enables a rapid, accurate and less labor-intensive approach to routine environmental 226Ra determination than the radioanalytical techniques conventionally applied.
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- 2007
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41. Introducing wet aerosols into the static high sensitivity ICP (SHIP)
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Andy Scheffer, Wolfgang Buscher, Carsten Engelhard, and Michael R. Sperling
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Torch ,Argon ,Chemistry ,Analytical chemistry ,chemistry.chemical_element ,Plasma ,Injector ,Biochemistry ,Analytical Chemistry ,law.invention ,Volumetric flow rate ,Aerosol ,Nebulizer ,law ,Inductively coupled plasma - Abstract
A demountable design of the static high sensitivity ICP (SHIP) for optical emission spectrometry is presented, and its use as an excitation source with the introduction of wet aerosols was investigated. Aerosols were produced by standard pneumatic sample introduction systems, namely a cross flow nebulizer, Meinhard nebulizer and PFA low flow nebulizer, which have been applied in conjunction with a double pass and a cyclonic spray chamber. The analytical capabilities of these sample introduction systems in combination with the SHIP system were evaluated with respect to the achieved sensitivity. It was found that a nebulizer tailored for low argon flow rates (0.3-0.5 L min(-1)) is best suited for the low flow plasma (SHIP). An optimization of all gas flow rates of the SHIP system with the PFA low flow nebulizer was carried out in a two-dimensional way with the signal to background ratio (SBR) and the robustness as optimization target parameters. Optimum conditions for a torch model with 1-mm injector tube were 0.25 and 0.36 L min(-1) for the plasma gas and the nebulizer gas, respectively. A torch model with a 2-mm injector tube was optimized to 0.4 L min(-1) for the plasma gas and 0.44 L min(-1) for the nebulizer gas. In both cases the SHIP system saves approximately 95% of the argon consumed by conventional inductively coupled plasma systems. The limits of detection were found to be in the low microgram per litre range and below for many elements, which was quite comparable to those of the conventional setup. Furthermore, the short-term stability and the wash out behaviour of the SHIP were investigated. Direct comparison with the conventional setup indicated that no remarkable memory effects were caused by the closed design of the torch. The analysis of a NIST SRM 1643e (Trace Elements in Water) with the SHIP yielded recoveries of 97-103% for 13 elements, measured simultaneously.
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- 2007
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42. Combined use of total metal content and size fractionation of metal biomolecules to determine the provenance of pine nuts (Pinus pinea)
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José Luis Gómez-Ariza, Tamara García-Barrera, and Ana Arias-Borrego
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Provenance ,Macromolecular Substances ,Size-exclusion chromatography ,Biocompatible Materials ,Fractionation ,Mass spectrometry ,Biochemistry ,Chemistry Techniques, Analytical ,Mass Spectrometry ,Analytical Chemistry ,Gel permeation chromatography ,Nuts ,Chromatography ,Manganese ,Principal Component Analysis ,Chemistry ,Reproducibility of Results ,Hydrogen-Ion Concentration ,Solutions ,Models, Chemical ,Metals ,Environmental chemistry ,Principal component analysis ,Spectrophotometry, Ultraviolet ,Composition (visual arts) ,Inductively coupled plasma ,Chromatography, Liquid - Abstract
Four essential elements (Mn, Ni, Zn, and Cu) and their molecular-size distribution patterns have been determined, for twenty four samples of pine nuts from eight areas in Spain and Portugal (Huelva, Cádiz, Badajoz, Cataluña, Castilla, Madrid, Faro, and Coimbra), by size-exclusion liquid chromatography (SEC) coupled on-line to UV and inductively coupled plasma mass spectrometric (ICP-MS) detection. The variability observed in total element content and the size-exclusion profiles of elements in samples from distant areas were considered as chemical descriptors for characterization of geographic origin. A pattern-recognition technique, the display method principal component analysis, was used as visualization technique to determine the provenance of the pine nuts collected. The results obtained confirmed that size fractionation profiles give more information for assessing the provenance of pine nuts than the total elements composition traditionally used for this purpose. Combination of these chemical descriptors was the most suitable choice for the samples studied. Figure This paper shows the application of an analytical approach based on total elements concentrations and the relative abundance of metal-biomolecules, estimated by the size-exclusion fractions, as chemical descriptors to determine the provenance of pine nuts. Principal component analysis (PCA) has been used as a visualization technique.
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- 2007
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43. Determination of lead in blood by laser ablation ICP-TOF-MS analysis of blood spotted and dried on filter paper: a feasibility study
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James V. Cizdziel
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Analytical chemistry ,Biochemistry ,Analytical Chemistry ,Humans ,Mass Screening ,Sample preparation ,Child ,Whole blood ,Venipuncture ,Chromatography ,Laser ablation ,Filter paper ,Chemistry ,Lasers ,Spectrophotometry, Atomic ,Reference Standards ,Contamination ,United States ,Lead Poisoning ,Freeze Drying ,Blood Stains ,Lead ,Microscopy, Electron, Scanning ,Feasibility Studies ,Inductively coupled plasma ,Quantitative analysis (chemistry) - Abstract
Screening programs for pediatric lead (Pb) poisoning routinely collect blood by finger stick onto specially designed filter paper (FP) for subsequent laboratory testing. Here, laser ablation inductively coupled plasma time-of-flight mass spectrometry is evaluated as a novel method for the determination of Pb in blood spotted onto FP cards. The method requires no sample pretreatment and may be particularly suitable for rapidly screening a large number of samples. Signal intensity from the ICP-MS strongly correlated (r (2) = 0.996) with Pb target values for five blood cards from a laboratory proficiency testing program. Better precision was obtained by replicate ablation line scans (15% rsd) compared to a grid of 25 individual ablation spots (30% rsd). Because2% of the sample is consumed in the laser ablation analysis, selected samples can also be analyzed by traditional techniques or archived. Lead isotope ratios determined during the same total-Pb analysis appear to be effective for discerning contamination extraneous to the blood sample. Determining that an elevated result was due to contamination may negate the need for retesting with invasive pediatric venipuncture. Some elements monitored along with Pb exhibited signal profiles conducive to potential quantitation (Ca, V, Fe, Cu Zn), whereas others did not (Cr, Mn, Co, Ni, Cd, Hg, Tl, U). Copper, Ca, and V were inversely correlated with Pb (r = -0.89, -0.90, and -0.92, respectively). Scanning electron microscope images revealed surface modality differences between FP spotted with fresh whole blood and reconstituted freeze-dried blood reference material.
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- 2007
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44. Assessment of chemical purity of 10B-enriched p-boronophenylalanine by high-performance liquid chromatography coupled on-line with inductively coupled plasma optical emission spectrometry
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Marı́a J Roberti, Eduardo A. Gautier, Raúl Jiménez Rebagliati, Daniel A. Batistoni, and Raquel T. Gettar
- Subjects
Boron Compounds ,Detection limit ,Radiation-Sensitizing Agents ,Chromatography ,Resolution (mass spectrometry) ,Chemistry ,Elution ,Phenylalanine ,chemistry.chemical_element ,Reversed-phase chromatography ,Buffers ,Hydrogen-Ion Concentration ,Biochemistry ,High-performance liquid chromatography ,Analytical Chemistry ,Drug Stability ,Spectrophotometry ,Impurity ,Tyrosine ,Spectrophotometry, Ultraviolet ,Inductively coupled plasma ,Boron ,Chromatography, High Pressure Liquid - Abstract
A dual-detection technique, consisting of a combination of reversed-phase high-performance liquid chromatography and on-line detection of elemental boron in the column effluents by inductively coupled plasma optical emission spectrometry, was tested for drug analysis. The method was applied to assessing the chemical purity of p-boronophenylalanine (BPA), isotopically enriched in 10B. This compound is employed as a fructose complex solution for biodistribution studies in laboratory and clinical trials of boron neutron capture therapy. Besides the determination of the content of BPA, required for chemical quality controls of solutions of the complex used for infusions, resolution of mixtures of BPA and two usually accompanying residual impurities (phenylalanine and tyrosine) was achieved with UV detection. The limits of detection (in solution) were 1.5 and 0.6 ng ml-1, respectively. In addition, by monitoring a sensitive-element emission wavelength it was possible to jointly observe the elution of boron-containing compounds that may be transparent to UV radiation or to confirm the presence of boron in potential impurities accompanying the drug. Those impurities may arise from the BPA synthesis or may be produced by degradation during the aging of the solutions. Chromatographic peaks corresponding to the amino acids and also to a related inorganic compound were detected in BPA-fructose complex solutions that were stored for different times and under different conditions. An increase in the areas of the peaks attributed to tyrosine and phenylalanine was observed for BPA-fructose solutions stored refrigerated for 1 month to 1 year, suggesting that degradation processes able to reduce the amount of bioavailable BPA could be active.
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- 2007
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45. Determination of major and trace elements in human scalp hair by pressurized-liquid extraction with acetic acid and inductively coupled plasma–optical-emission spectrometry
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Antonio Moreda-Piñeiro, Elia Alonso-Rodríguez, Jorge Moreda-Piñeiro, Darío Prada-Rodríguez, Pilar Bermejo-Barrera, Soledad Muniategui-Lorenzo, and Purificación López-Mahía
- Subjects
Detection limit ,Scalp ,Chromatography ,Chemistry ,Temperature ,Analytical chemistry ,Reproducibility of Results ,Repeatability ,Elements ,Mass spectrometry ,Diatomaceous Earth ,Biochemistry ,Trace Elements ,Analytical Chemistry ,Certified reference materials ,Spectrophotometry ,Liquid–liquid extraction ,Inductively coupled plasma atomic emission spectroscopy ,Pressure ,Humans ,Sample preparation ,Particle Size ,Inductively coupled plasma ,Acetic Acid ,Hair - Abstract
An analytical method has been developed for determination of major (Ca, K, Mg, and Na) and trace elements (As, Cd, Co, Li, Ni, and Sr) in human scalp hair. The proposed method includes a novel, simple, rapid, highly efficient, and automated metal-leaching procedure, by pressurized-liquid extraction (PLE), combined with a rapid simultaneous detection system-inductively coupled plasma-optical-emission spectrometry (ICP-OES). PLE is one of the most promising recently introduced sample-preparation techniques, with the advantages of reducing solvent consumption and enabling automated sample handling. The operating conditions for PLE, including concentration of the extraction solvent, extraction temperature, static time, number of extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio, and flush volume were studied using an experimental design (Plackett-Burman design, PBD). The optimum conditions were use of 0.75 mol L-1 acetic acid as extracting solution and powdered hair samples thoroughly mixed with DE, as a dispersing agent, at a DE mass/sample mass ratio of 4. Extraction was performed at room temperature and an extraction pressure of 140 atm for 5 min in one extraction step. The flush volume was fixed at 60%. The PLE-assisted multi-element leaching proposed is complete after 7 min (5 min static time plus 1 min purge time plus 1 min end relief time). Under the optimised conditions the figures of merit, for example limits of detection and quantification, repeatability of the over-all procedure, and accuracy, were evaluated. Analysis of GBW-07601 (human hair) certified reference material revealed accuracy was good for the target elements. The optimised method was finally applied to several human scalp-hair samples.
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- 2007
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46. A matrix effect and accuracy evaluation for the determination of elements in milk powder LIBS and laser ablation/ICP-OES spectrometry
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Gilon, N., El-Haddad, J., Stankova, A., Lei, W., Ma, Q., Motto-Ros, V., and Yu, J.
- Published
- 2011
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47. Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review
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Marcia F. Mesko, Fabio A. Duarte, Juliano Smanioto Barin, Erico M.M. Flores, and Paola A. Mello
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Active ingredient ,Chromatography ,Chemistry ,010401 analytical chemistry ,02 engineering and technology ,Atomic spectroscopy ,Raw material ,021001 nanoscience & nanotechnology ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Dosage form ,Mass Spectrometry ,0104 chemical sciences ,Analytical Chemistry ,law.invention ,Pharmaceutical Preparations ,law ,Environmental chemistry ,Sample preparation ,Pharmacopoeia ,Inductively coupled plasma ,0210 nano-technology - Abstract
Interest in the determination of elemental impurities in pharmaceuticals has increased in recent years because of changes in regulatory requirements and the need for changing or updating the current limit tests recommended in pharmacopeias. Inductively coupled plasma (ICP) optical emission spectrometry and ICP mass spectrometry are suitable alternatives to perform multielemental analysis for this purpose. The main advantages and limitations of these techniques are described, covering the applications reported in the literature in the last 10 years mainly for active pharmaceutical ingredients, raw materials, and pharmaceutical dosage forms. Strategies used for sample preparation, including dissolution in aqueous or organic solvents, extraction, wet digestion and combustion methods are described, as well as direct solid analysis and ICP-based systems applied for speciation analysis. Interferences observed during the analysis of pharmaceutical products using ICP-based methods are discussed. Methods currently recommended by pharmacopeias for elemental impurities are also covered, showing that the use of ICP-based methods could be considered as a trend in the determination of these impurities in pharmaceuticals. However, the development of a general method that is accurate for all elemental impurities and the establishment of an official method are still challenges. In this regard, the main drawbacks and suitable alternatives are discussed.
- Published
- 2015
48. An in-depth evaluation of accuracy and precision in Hg isotopic analysis via pneumatic nebulization and cold vapor generation multi-collector ICP-mass spectrometry
- Author
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Frank Vanhaecke, Ana Rua-Ibarz, and Eduardo Bolea-Fernandez
- Subjects
Analyte ,Accuracy and precision ,Isotope ,Chemistry ,010401 analytical chemistry ,Analytical chemistry ,Fractionation ,Mercury ,010501 environmental sciences ,Mass spectrometry ,01 natural sciences ,Biochemistry ,Mass Spectrometry ,0104 chemical sciences ,Analytical Chemistry ,Isotopes ,Gases ,Inductively coupled plasma ,Volatilization ,Inductively coupled plasma mass spectrometry ,0105 earth and related environmental sciences ,Isotope analysis - Abstract
Mercury (Hg) isotopic analysis via multi-collector inductively coupled plasma (ICP)-mass spectrometry (MC-ICP-MS) can provide relevant biogeochemical information by revealing sources, pathways, and sinks of this highly toxic metal. In this work, the capabilities and limitations of two different sample introduction systems, based on pneumatic nebulization (PN) and cold vapor generation (CVG), respectively, were evaluated in the context of Hg isotopic analysis via MC-ICP-MS. The effect of (i) instrument settings and acquisition parameters, (ii) concentration of analyte element (Hg), and internal standard (Tl)-used for mass discrimination correction purposes-and (iii) different mass bias correction approaches on the accuracy and precision of Hg isotope ratio results was evaluated. The extent and stability of mass bias were assessed in a long-term study (18 months, n = 250), demonstrating a precision ≤0.006% relative standard deviation (RSD). CVG-MC-ICP-MS showed an approximately 20-fold enhancement in Hg signal intensity compared with PN-MC-ICP-MS. For CVG-MC-ICP-MS, the mass bias induced by instrumental mass discrimination was accurately corrected for by using either external correction in a sample-standard bracketing approach (SSB) or double correction, consisting of the use of Tl as internal standard in a revised version of the Russell law (Baxter approach), followed by SSB. Concomitant matrix elements did not affect CVG-ICP-MS results. Neither with PN, nor with CVG, any evidence for mass-independent discrimination effects in the instrument was observed within the experimental precision obtained. CVG-MC-ICP-MS was finally used for Hg isotopic analysis of reference materials (RMs) of relevant environmental origin. The isotopic composition of Hg in RMs of marine biological origin testified of mass-independent fractionation that affected the odd-numbered Hg isotopes. While older RMs were used for validation purposes, novel Hg isotopic data are provided for the latest generations of some biological RMs.
- Published
- 2015
49. Accurate purification age determination of individual uranium-plutonium mixed particles
- Author
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Fumitaka Esaka, Yutaka Miyamoto, Masaaki Magara, and Daisuke Suzuki
- Subjects
Isotope ,Chemistry ,Ion chromatography ,Radiochemistry ,Analytical chemistry ,chemistry.chemical_element ,Uranium ,Mass spectrometry ,Biochemistry ,Analytical Chemistry ,Plutonium ,Certified reference materials ,Inductively coupled plasma ,Inductively coupled plasma mass spectrometry - Abstract
Age of individual uranium-plutonium (U/Pu) mixed particles with various U/Pu atomic ratios (1-70) were determined by inductively coupled plasma mass spectrometry. Micron-sized particles were prepared from U and Pu certified reference materials. The Pu reference was stored for 4-6 years since the last purification (July 14, 2008). The Pu purification age was obtained from the (241)Am/(241)Pu ratio which was calculated from the product of three measured ratios of Pu and Am isotopes in the eluted fractions. These ratios were measured by a high-resolution inductively coupled plasma mass spectrometer equipped with a desolvation system. Femto-gram to pico-gram quantities of Am, U, and Pu in a sample solution were sequentially separated on a small anion-exchange column. The (241)Am/(241)Pu ratio was accurately determined by spiking pure (243)Am into the sample solution. The average determined age for the particles for the five independent U/Pu ratios was in good agreement with the expected age with high accuracy (difference age 0.27 years) and high precision (standard deviation 0.44 years). The described analytical technique can serve as an effective tool for nuclear safeguards and environmental radiochemistry. Figure Young (4-6 y) Pu purification age of individual U/Pu mixed micron-sized reference particles for the five independent U/Pu ratios (1-70) were determined with 0.27±0.44 y difference from the expected age. Sub pico-gram quantities of Am, U and Pu were sequentially separated a small column, and their isotope ratios were accurately measured using an ICP-MS by applying the (243)Am spiking technique to the analysis and correcting the impurity and the contaminations.
- Published
- 2015
50. Spectrochemical plasmas for clinical and biochemical analysis
- Author
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Maria Montes-Bayón and Alfredo Sanz-Medel
- Subjects
chemistry.chemical_classification ,Clinical Laboratory Techniques ,Biomolecule ,Context (language use) ,Plasma ,Mass spectrometry ,Biochemistry ,Mass Spectrometry ,Analytical Chemistry ,chemistry ,Separation method ,Humans ,Protein activity ,Biochemical engineering ,Inductively coupled plasma ,Optical emission spectrometry - Abstract
Plasma-based analytical strategies have been used in the context of elemental detection (total elemental determination) in biochemical and clinical samples for a number of years. But the applicability of these detection methods to more sophisticated analytical problems associated with the use, for instance, of new metallodrugs as therapeutic agents in different kinds of diseases or the interest in the fate of metallic nanoparticles in biochemical environments has reactivated the use of plasma-based methods in the bioworld. Thus, the state of the art of metal-derived information obtained in biological and clinical samples using plasma-based strategies has been the driving force for this special issue. In this regard, from examination of the contributions to this issue, the first conclusion that can be drawn is that although element-specific detection can be conducted using a plethora of plasma techniques (a review on dielectric barrier discharge is included in this issue), inductively coupled plasma (ICP) mass spectrometry (MS) is still the most widely used detection method for bioapplications. The analytical advantages of ICP-MS over other elemental detection methods based on photon measurement (e.g., atomic absorption spectrometry or ICP optical emission spectrometry) are well known, and are mainly ascribed to the extremely high sensitivity of the technique together with its capability to measure isotopes and isotopic ratios, making possible screening and speciation of very low levels of heteroatoms in biomolecules or biological tissues. This fact has been exploited in some of the work reported in this issue for biosamples in combination with different separation methods necessary in order to achieve the desired species purity or directly on the tissues by applying laser ablation techniques. Secondly, an interesting feature observed in the articles of this issue is the “quantitative” dimension of the work realized. Most articles contain quantitative elemental data and try to correlate themwith species information (in the case of having these heteroelements as part of metabolites or proteins) or element/ drug distribution in tissues (imaging) by sorting with different quantification strategies. In this context, it is possible to address that plasma-based analysis becomes quantitative by providing a variety of strategies for absolute quantifications of low levels of the target heteroatoms in biological samples. In addition, it is noteworthy that the trend in some articles to combine the elemental information (provided by the corresponding plasma-based strategy) with specific biological information— for example, protein activity or DNA–protein interaction—has been rarely addressed so far using ICP-MS. It may be that novel future uses of plasma technology go in this direction. Lastly, regarding the topics of research chosen, it is possible to observe the increasing use of plasma-based strategies to address the fate of heteroelement-containing drugs in different biological samples or their consequences. It seems clear that the excellent analytical features provided by ICP-MS, in particular for monitoring platinumcontaining drugs of extended use in chemotherapy, have now been favorably used also for monitoring gadolinium Published in the topical collection Spectrochemical Plasmas for Clinical and Biochemical Analysis with guest editors Alfredo Sanz-Medel and Maria Montes Bayon. M. Montes-Bayon (*) :A. Sanz-Medel Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, C/ Julian Claveria 8, 33006 Oviedo, Spain e-mail: montesmaria@uniovi.es
- Published
- 2015
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