107 results on '"Liquid liquid extraction"'
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2. Sütte Glukokortikoidlerin analizi için metot karşılaştırması.
- Author
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Dudaklı, Gülay and Vural, Handan
- Abstract
Copyright of Etlik Veteriner Mikrobiyoloji Dergisi is the property of Veteriner Kontrol Merkez Arastirma Enstitusu and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
- Published
- 2024
- Full Text
- View/download PDF
3. Editorial: Separation and analytical chemistry
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Pankaj Kumar Parhi
- Subjects
ionic liquid ,liquid liquid extraction ,green chemistry ,metal ,extraction ,Chemistry ,QD1-999 - Published
- 2023
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4. Bioprocessing of bacteriophages and bacteriocins : continuous culture and downstream purification
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Mancuso, Francesco
- Subjects
660.6 ,bacteriophages ,phages ,fermentation ,upstream ,downstream ,bioprocessing ,Recombinant Proteins Produced ,Colicin E9 Expression ,Continuous Culture ,synthetic media ,chemically defined media ,Tangential Flow Ultrafiltration ,Cross Flow Ultrafiltration ,chromatography purification step ,Ion Exchange Chromatography ,size exclusion ,liquid liquid extraction ,octanol phase ,endotoxin lipopolysaccharide ,LPS ,Diafiltration ,NTA - Abstract
Antimicrobial resistance poses a major problem to health and new alternatives to antibiotics are required. Bacteriophages are viruses able to selectively kill bacteria and they can be exploited to treat infections. Another alternative to antibiotics that can be used to treat bacterial infections are bacteriocins, which are proteins produced by bacteria, meant to kill other strains competing for the same nourishment source. Future industrial demand for large quantities of bacteriophages and bacteriocins imposes the development of a scalable production platform. In this PhD thesis, research on bioprocessing of bacteriophages K and T3 and one bacteriocin belonging to the subcategory of colicins, E9, has been conducted. The aims were to find the parameters involved in production of phages and colicin E9 using shake flasks and then exploiting them to perform continuous production of both phages and colicin E9 and showing the different outcomes when using complex medium (LB) and a synthetic medium (SM) using glucose as only carbon source. For the colicin E9 bioprocessing, tests for expression were carried out to measure when and for how long to induce for optimal protein production and the best conditions for production were an induction of 3 h with 1 mM of IPTG in LB medium and >10 h of induction with 1 mM of IPTG in SM. These parameters were used for continuous production of colicin E9 that was carried out using a chemostat. Optimal dilution rates were used to ensure maximum productivity and a production of 1 mg mL-1 of colicin E9 was achieved using either LB and synthetic medium. Then, the influence of flowrates and of different growth media on the first step of purification was assessed using affinity chromatography, showing that the synthetic medium allowed higher recovery of the product in the chromatography step. Bioprocessing of the phages K and T3 was carried out in shake flasks and 5L fermenters, researching the best parameters for producing the highest titres. The effect on the final titre of a variety of multiplicities of infection (MOI), the ratio of phages out of bacteria at the moment of infection, was evaluated. For both phages the MOI that ensured the highest phage titre, 1011 PFU mL-1, was 0.01. The parameters measured were then used for continuous production of bacteriophage T3. Continuous phage T3 production was carried out using a novel reactors layout, composed by 3 separated stages. This set up allowed to divide the production of the host cells, carried out in the first reactor, from the infection, carried out in the second reactor, and from the final amplification step, carried out in the third reactor. The synthetic medium with glucose as only carbon source and the dilution rate (D, the volume of media that flows in the reactor per hour) were used to control the growth rate of the host, which strongly influenced the final production of bacteriophages. Different D iii were tested, from 0.1 to 0.6 h-1 and the independent control of the dilution rate of the first and the second reactor allowed to produce phage lysates at the same concentrations as in batch process, reaching a constant production of 2x1011 PFU mL-1 when D = 0.5 h-1 was used in the first reactor. Moreover, research on the downstream process of phage bioprocessing was conducted, aiming to reduce the host cell protein burden from phage samples using scalable techniques. The purification of bacteriophages from complex medium was performed using ultrafiltration in batch mode in a stirred cell (SC) and in using tangential flow filtration (TFF). The high shear stress produced SC decreased the viability of the tailed phage K of 2 log10 in 2 h and the positive effects of purification were cancelled by the loss of titre. Phage T3, which has a short tail, showed no side effects due to shear stress. TFF was then tested and both phage K and T3 were purified without significant viability loss. Size exclusion chromatography was used to assess the final protein concentration and showed a decrease of host cell protein load in both phages samples purified by ultrafiltration. Samples of both phages were mixed with a positively charged resin used for anion exchange chromatography and it was shown that phages that have been filtered using ultrafiltration can bind 10 times more than phages of the lysate. The main aim of purification phages produced from Gram-negative bacteria, such as T3, was to reduce the endotoxin levels (or lipopolysaccharide, LPS). Endotoxins are a major contaminant that can cause serious problems if administered and must be removed from drug products. The target was to bring the LPS levels from the initial concentration of 5x106 EU mL-1 (Endotoxin Units per mL) below the limit of 5 EU mL-1. Endotoxin removal was performed using ultrafiltration and liquid-liquid extraction (LLE). The first method tested was the TFF ultrafiltration, carried out in batch mode or in diafiltration mode. Batch ultrafiltration showed a decrease of LPS of 2 log10, either starting from a phage T3 sample from LB or from SM. Diafiltration TFF reached 3 log10 reduction of LPS in both LB or SM samples, but in LB samples it took 20 h and in SM samples only 4 h, showing how a chemically defined medium could improve the purification of phages produced from Gram-negative hosts. The other method tested to further reduce LPS concentration was liquid-liquid extraction, using 1- octanol as organic phase. Many different conditions of LLE were tested, such as length of contact time between aqueous and organic phases, different mixing methods and number of extractions. Liquid- liquid extraction using octanol ensured a reduction of endotoxins of 4 log10 from the initial concentration. This technique was then followed by ion exchange chromatography, which allowed to reach a final concentration of 102 EU mL-1. Finally, analysis on how endotoxins concentrations affected the aggregation of phage T3 were performed, showing how phage T3 aggregates in presence of endotoxins whilst it has a low polidspersivity at low endotoxins concentrations. This thesis showed how is it possible to produce bacteriophages and an antimicrobial protein at high concentrations using a continuous production mode and a chemically defined medium. The positive effects of the synthetic medium on the downstream steps were also illustrated, such as a lower burden for ion exchange columns and a faster reduction of endotoxin concentration from the samples.
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- 2019
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5. 高效液相色谱-串联质谱法和高效液相色谱法测定 蜂蜜中氯虫苯甲酰胺残留量.
- Author
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梁 宇, 司露露, 汪文龙, 黄 恺, 蔡翔宇, 苏 华, and 秦 富
- Abstract
Copyright of Journal of Food Safety & Quality is the property of Journal of Food Safety & Quality Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
- Published
- 2022
6. Separation and Preconcentration Methods (Excluding Chromatography)
- Author
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Zolotov, Yury A. and Zolotov, Yury A.
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- 2018
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7. Distribution of different no-carrier-added radionuclides in Pb and Bi fractions after separation of bulk components of lead bismuth eutectic.
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Choudhury, Dibyasree, Naskar, Nabanita, and Lahiri, Susanta
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RADIOISOTOPES , *BISMUTH , *PROTON beams , *GALLIUM alloys , *GADOLINIUM - Abstract
Large numbers of radionuclides are produced when 1.4 GeV proton beam hits lead bismuth eutectic (LBE) target. Separation of desired radionuclide from large amount of bulk components and other co-produced radionuclides is a challenging task. In this experiment, such a case has been simulated by irradiating a LBE target with low energy proton beam and spiked with nine radionuclides (56Co, 67 Ga, 90Nb, 149Gd, 157Dy, 172Lu, 182Re, 195mHg, 198Tl). The bulk Pb and bulk Bi were separated from irradiated LBE target matrix by different methods and the distribution pattern of these radionuclides were studied in the separated Pb and Bi fraction. [ABSTRACT FROM AUTHOR]
- Published
- 2021
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8. Reversible dye extraction from aqueous matrices using ammonium salt-based deep eutectic solvents.
- Author
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Martínez-Rico, Óscar, Asla, Andrés, Domínguez, Ángeles, and González, Begoña
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EUTECTICS , *AMMONIUM salts , *DYES & dyeing , *WATER reuse , *SOLVENTS , *LIQUID-liquid equilibrium , *LIQUID-liquid extraction , *DECANOIC acid - Abstract
• Ammonium salt-based Deep Eutectic Solvents are good extractants for textile dyes. • Characteristic functional groups in dyes can be targeted to enhance extraction. • The reuse of the cleaned water and of the extracted dye is possible. • Simulated effluents composed by industrial dyes are treated. Recovery of dyes present in liquid solutions was achieved with efficiencies higher than 99 %, using deep eutectic solvents composed of tetrabutylammonium chloride and decanoic acid. The method produces a totally decolorized water. Both the reuse of the clean water and of the extracted dye is plausible via this treatment, as the colorant can be recovered from the organic phase after the liquid–liquid extraction. The solvent is physically and chemically characterized, in a wide arrange of temperatures, and its behavior in liquid–liquid equilibria with water was also studied. The process works for a broad range of dye concentrations, and with a very low consumption of solvent (optimized volumetric ratio between organic and aqueous phases was 1/16). Optimized processing times set the duration of the treatment at 20 min, including the recovery of the dye from the extracted phase. The capabilities of the solvent were tested against synthetic effluents composed by industrial dyes and auxiliary agents that typically appear on dyeing processes, maintaining efficiencies above 99 %. The deep eutectic solvents also work equally well for extracting mixtures of dyes. [ABSTRACT FROM AUTHOR]
- Published
- 2024
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9. Extraction of Metronidazole and Furazolidone from industrial effluents by double salting out assisted liquid liquid extraction technique and their analyses by HPLC-UV method.
- Author
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Bukhari, Syed Waqas and Ansari, Tariq Mahmood
- Abstract
We have developed a new analytical method for simultaneous determination of Metronidazole and Furazolidone by High Performance Liquid Chromatography (HPLC). The method is coupled to double salting-out assisted liquid-liquid extraction (SALLE) which facilitates the detection and quantification of Metronidazole and Furazolidone in different dosage forms by subsequent HPLC analysis. Extraction parameters such as solvent, pH and salt concentration are optimized and liquid liquid extraction showed efficiency up to 102% and 100% for Metronidazole and Furazolidone respectively in chloroform, at pH 3 and low salt concentration (0.5g KCl and 0.5 gNaNO
3 ). The designed simultaneous analytical method is further validated and Metronidazole and Furazolidone showed linearity upto R²0.994 and 0.9936 respectively. LOD was 2.1µg/ml, 1.5µg/ml and LOQ was 21.1µg/ml, 15.2µg/ml for metronidazole benzoate and furazolidone. Precision of the method is 1.84% (RSD) and 1.72% (RSD) for Metronidazole and Furazolidine respectively. Moreover, accuracy is measured in terms of percent recovery which is more than 100% for both analytes under optimized conditions. Finally, robustness is evaluated by changing the flow rate and detection wavelength which is also obtained within permissible limit. This indicates that the proposed method is simple, efficient and shows excellent recoveries for simultaneous determination of Metronidazole and Furazolidone in different dosage forms and Industrial effluents. [ABSTRACT FROM AUTHOR]- Published
- 2020
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10. Validation of an Analytical Method for Simultaneous Determination of 18 Persistent Organic Pollutants in Trout Using LLE Extraction and GC-MS/MS.
- Author
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Bayat, Mitra, tehrani, Mohammad Saber, Kobarfard, Farzad, Husain, Syed Waqif, and Yazdanpanah, Hassan
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PERSISTENT pollutants , *ORGANOCHLORINE pesticides , *TROUT , *HAZARDOUS substances , *AQUATIC animals , *STANDARD deviations , *METHOXYCHLOR - Abstract
Persistent organic pollutants, (POPs), are vast distributed compounds in environment which are recognized as one of the global pollution problems. These groups of materials being dangerous due to their high stability are accumulated in animal tissues and occurring in the food chain. One of the major paths through which persistent organic combinations access to human body is consuming polluted foods, particularly, fishes. Among aquatic animals, trout as one of the mostly consumed fishes in Tehran's food basket was studied. In this study, two categories of persistent organic pollutants: Organochlorine pesticides (OCPs) including HCB, Dieldrin, Methoxychlor, α-, ϒ-Chlordane, α-, β-Endosulfan and o,p'-DDE, p,p'-DDE, o,p'- DDT, p,p'-DDT and the second group Polychlonitated biphenyls (PCBs) including seven PCB congeners which are called indicator PCBs (IUPAC nos.: 28,52,101,118,138,153 and 180) were determined in trout by GC-MS/MS in MRM monitoring mode and LLE extraction. The average recoveries of OCPs and PCBs at five concentration levels (1, 2, 5, 10 and 20 ng/g for PCBs and 5 times for OCPs) were in the range of 73-112%. The relative standard deviations of POPs in fish were in the range of 1.4-17.9% for all of the concentration levels. The limit of detections (LODs) and the limit of quantitations (LOQs) were between 0.6-8.3 and 2-25 μg/kg, respectively. The results indicated the presence of organochlorine pesticides in trout and the levels of p,p'-DDE and p,p'-DDT were within the range of < LOQ -12.83 and < LOQ -10.2 ng/g ww (wet weight), respectively. According to the results, OCPs residues were lower than maximum residue levels set by European Council Directives. [ABSTRACT FROM AUTHOR]
- Published
- 2019
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11. Decolorization of synthetic textile effluents using methyltrioctylammonium-based DES.
- Author
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Martínez-Rico, Óscar, Asla, Andrés, González, Begoña, and Domínguez, Ángeles
- Subjects
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SYNTHETIC textiles , *AMMONIUM chloride , *INDUSTRIAL wastes , *OCTANOIC acid , *LIQUID-liquid extraction - Abstract
[Display omitted] • Interactions with functional groups from the dye can be used to tailor solvents. • Methyltrioctylammonium salts play a key role to decolorize textile effluents. • Sodium groups present in dyes correlate to affinity with DESs. • Use of carboxylic acids result in DESs with manageable physical properties. In light of the escalating environmental challenges posed by the huge generation of wastewater and residues from dyeing processes, addressing water scarcity concerns has become an urgent imperative. This study proposes a sustainable and environmentally friendly solution via liquid–liquid extraction to effectively eliminate dyes from industrial effluents, producing clean and reusable water resources. Methyltrioctylammonium (N 1888) based deep eutectic solvents (DESs) show remarkable capabilities as extracting agents. Combined with octanoic and decanoic acids, the bromide and chloride ammonium salts were used to prepare four solvents. They were physically characterized and tested before a wide variety of colorants and synthetic effluents, including real auxiliar agents used in the textile industry. Extraction percentages across all experiments showed an average of 98.39%, reaching a maximum of 99.96% efficiency for the extraction of Reactive Black 5 from aqueous solution, which shows the potential of these solvents to mitigate the environmental impact of dyeing processes. [ABSTRACT FROM AUTHOR]
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- 2024
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12. AN LC- MS/MS METHOD FOR THE DETERMINATION OF OMEPRAZOLE ON PROTON PUMP INHIBITOR IN HUMAN PLASMA
- Author
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T. Sudha, Kalan Kumar Reddy, P. V. Hemalatha, and V. R. Ravikumar
- Subjects
Proton pump inhibitor ,omeprazole ,lansoprazole ,LC-MS/MS ,liquid liquid extraction ,Pharmacy and materia medica ,RS1-441 - Abstract
A sensitive and selective liquid chromatographic method coupled with tandem mass spectroscopy (LC-MS/MS) was developed for the quantification of omeprazole in human plasma. Lansoprazole was used as internal standard with plasma samples, extracted using 10mM ammonium acetate. A centrifuged upper layer was then evaporated and reconstituted with Acetonitrile: mobile phase buffer 70:30%v/v. The reconstructed samples were injected into a C18 column purospher star 5µ. The mobile phase was composed of ACN: mobile phase buffer (5mm ammonium bicarbonate buffer) in the ratio of 70:30%v/v with flow rate 1.0mL/min. The mass spectrometer was operated using positive ion mode and turbo electro spray ionisation. Nitrogen was used as the nebulizer, curtain, collision and auxiliary gases. Using MS/MS with multiple reactions monitoring (MRM) mode, omeprazole was detected without severe interferences from plasma matrix. Detection of omeprazole in human plasma was accurate and precision. This method has been successfully applied to the study of omeprazole in human specimens
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- 2016
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13. An Amperometric Sensor for the Selective Determination of Ortho-Diphenols in Olive Oil
- Author
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Del Carlo, Michele, Pepe, Alessia, Della Pelle, Flavio, Mascini, Marcello, Compagnone, Dario, Amine, Aziz, Kadi, Azedin, Amraoui Bendriss, Nora, Fusella, Giuseppe Christian, Neri, Giovanni, editor, Donato, Nicola, editor, d'Amico, Arnaldo, editor, and Di Natale, Corrado, editor
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- 2011
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14. UNIFAC Group Interaction Prediction for Ionic Liquid-Thiophene Based Systems Using Genetic Algorithm
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Singh, Surya Pratap, Anantharaj, Ramalingam, Banerjee, Tamal, Hutchison, David, Series editor, Kanade, Takeo, Series editor, Kittler, Josef, Series editor, Kleinberg, Jon M., Series editor, Mattern, Friedemann, Series editor, Mitchell, John C., Series editor, Naor, Moni, Series editor, Nierstrasz, Oscar, Series editor, Pandu Rangan, C., Series editor, Steffen, Bernhard, Series editor, Sudan, Madhu, Series editor, Terzopoulos, Demetri, Series editor, Tygar, Doug, Series editor, Vardi, Moshe Y., Series editor, Weikum, Gerhard, Series editor, Deb, Kalyanmoy, editor, Bhattacharya, Arnab, editor, Chakraborti, Nirupam, editor, Chakroborty, Partha, editor, Das, Swagatam, editor, Dutta, Joydeep, editor, Gupta, Santosh K., editor, Jain, Ashu, editor, Aggarwal, Varun, editor, Branke, Jürgen, editor, Louis, Sushil J., editor, and Tan, Kay Chen, editor
- Published
- 2010
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15. Separation of Pb and Bi from proton irradiated lead-bismuth eutectic target using different anion exchangers.
- Author
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Choudhury, Dibyasree and Lahiri, Susanta
- Subjects
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EUTECTIC alloys , *LEAD-bismuth alloys , *SEPARATION (Technology) , *ION exchange (Chemistry) , *PROTON magnetic resonance - Abstract
Lead-bismuth eutectic (LBE) is the proposed material for use as converter targets in the ISOL facilities globally. In this paper, an LBE target was irradiated with 22 MeV proton beam for 7.6 h to produce 203,204,205,206Bi, 203Pb along with 207Po. Separation of bulk Pb and Bi has been carried out using Aliquat-336 (tricaprylmethylammonium chloride), TOA (trioctyl amine) and DOWEX-1 as extractants. Bi was selectively extracted to the organic/solid phase leaving Pb in aqueous medium. High separation factor between Pb and Bi was observed when 0.5 M TOA and 1 M HNO3 were used as organic and aqueous phase respectively. [ABSTRACT FROM AUTHOR]
- Published
- 2018
- Full Text
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16. Method development and validation for estimation of Felodipine in human plasma by LCMS/MS
- Author
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Reddy, Srinivas, Joseph, Jibin V., Kumar, Aravind, Mukhopadhyay, Arindam, and Thangam, Saral
- Published
- 2013
17. Synthesis, characterization, and metal-ion binding properties of a new macrobicyclic ligand with dioxadiazaoctathia donor atoms.
- Author
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Gök, Halil Zeki and Gök, Yaşar
- Subjects
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METAL ions , *LIQUID-liquid extraction , *SPECTROMETRY , *DICHLOROMETHANE , *CHLOROFORM - Abstract
In this study, a new macrobicyclic ligand 3 with mixed donor atoms was synthesized starting from 27-membered macrocycle ligand 1 via the formation of novel N-pivot lariat ether 2. The characterization of the structures of new compounds 2 and 3 was realized by several spectroscopic techniques such as 1H NMR, 13C NMR, IR, UV-Vis, and MS. Besides, the extraction ability of ligands 2 and 3 was investigated using liquid-liquid extraction. On considering the extraction, the highest efficiency was observed for Ag(I) ion by 95.3% and 96.9% to the dichloromethane and chloroform phase with macrobicyclic ligand 3, respectively. [ABSTRACT FROM AUTHOR]
- Published
- 2017
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18. Inter-laboratory validation of a thin film microextraction technique for determination of pesticides in surface water samples.
- Author
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Piri-Moghadam, Hamed, Gionfriddo, Emanuela, Rodriguez-Lafuente, Angel, Grandy, Jonathan J., Lord, Heather L., Terry Obal, and Pawliszyn, Janusz
- Subjects
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THIN films , *PESTICIDES , *WATER , *SEPARATION (Technology) - Abstract
The primary goal of the present study is the inter-laboratory evaluation of a thin film microextraction (TFME) technique to be used as an alternative approach to liquid-liquid extraction (LLE). Polydimethylsiloxane/divinylbenzene (PDMS/DVB) and PDMS/DVB-carbon mesh supported membranes were used for the extraction of 23 targeted pesticides, while a thermal desorption unit (TDU) was employed to transfer these analytes to a GC/MS instrument for separation and detection. After optimization of the most critical parameters, both membranes were capable of achieving limits of detection (LOD) in the low ng L-1 range while demonstrating excellent robustness, withstanding up to 100 extractions/desorption cycles. Furthermore, limits of quantification (LOQ) between 0.025 and 0.50 μg L-1 were achieved for the 23 compounds selected from several classes of pesticides with a wide range of polarities. A wide linear range of 0.025-10.0 μg L-1 with strong correlation to response (R2 > 0.99) was attained for most of the studied analytes. Both membranes showed good accuracy and repeatability at three levels of concentration. Moreover, the method was also validated through blind split analyses of 18 surface water samples, collected within 3 months, using TFME at the University of Waterloo and LLE at Maxxam Analytics (Mississauga, ON) which is an accredited commercial analytical laboratory. Good agreement between the two methods was achieved with accuracy values ranging from 70 to 130%, for the majority of analytes in the samples collected. At the concentration levels investigated, 90% of the analytes were quantifiable by TFME, whereas only 53% of the compounds were reportable using the LLE method particularly at concentrations lower than 1 μg L-1. The comparison of TFME and LLE from several analytical aspects demonstrated that the novel TFME method gave similar accuracy to LLE, while providing additional advantages including higher sensitivity, lower sample volume, thus reduced waste production, and faster analytical throughput. Given the sensitivity, simplicity, low cost, accuracy, greenness and relatively fast procedure of TFME, it shows great potential for adoption in analytical laboratories as an alternative to LLE. [ABSTRACT FROM AUTHOR]
- Published
- 2017
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19. Phosphorylated Cavitands: Encapsulation of Hard Cationic Guests
- Author
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Delangle, Pascale, Mulatier, Jean-Christophe, Dutasta, Jean-Pierre, and Coleman, A. W., editor
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- 1998
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20. Mechanism analysis of liquid-liquid extraction separation for dimethyl carbonate and methanol by choline-based DESs as extractants.
- Author
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Yin, Kexin, Shen, Yuanyuan, Jiao, Yuyang, Zhou, Mengjin, Wang, Xianlong, Zhu, Zhaoyou, Cui, Peizhe, and Wang, Yinglong
- Subjects
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LIQUID-liquid extraction , *CHOLINE chloride , *QUANTUM chemistry , *DIFFUSION coefficients , *RADIAL distribution function , *ETHANES - Abstract
Dimethyl carbonate (DMC) is a widely used chemical raw material and chemical product with excellent performance. In this manuscript, based on electrostatic potential (ESP), reduced density gradient (RDG) function, non-bond interaction energy, radial distribution function (RDF), spatial distribution function (SDF) and self-diffusion coefficient, the separation of DMC / methanol (MeOH) by four deep eutectic solvents (DESs) was studied. The results of ESP analysis showed that the hydrogen bond receptor played a leading role in the separation process, and the urea in the four hydrogen bond donors was more likely to form a stable structure with MeOH. The weak interaction region between different DESs and azeotropes was studied by RDG function. Based on the non-bond interaction energy, it can be seen that Cl− can form a very strong interaction with MeOH, and Electrostatic energy (E elec) plays a leading role in the separation process. The charge density around the central atom can be observed by RDF and SDF, so as to determine the interaction between azeotrope and DESs. The diffusion rate of azeotrope in different DESs was studied by self-diffusion coefficient. The results showed that MeOH moved the slowest in the DES composed of urea and choline chloride (CHCl). The effect of DES structure on the liquid level of methanol dimethyl carbonate system was clarified by analyzing the experimental liquid-liquid equilibrium data. In this study, based on quantum chemistry (QC) calculation and molecular dynamics (MD) simulation, this study analyzed the liquid-liquid extraction and separation mechanism of DMC and MeOH. The extraction effect of DES composed of CHCl+urea is the best, which has certain theoretical guiding significance for liquid-liquid extraction to realize the green and efficient separation of DMC and MeOH. [ABSTRACT FROM AUTHOR]
- Published
- 2023
- Full Text
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21. Development and optimization of ultra-high performance supercritical fluid chromatography mass spectrometry method for high-throughput determination of tocopherols and tocotrienols in human serum.
- Author
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Pilařová, Veronika, Gottvald, Tomáš, Svoboda, Pavel, Novák, Ondřej, Benešová, Karolína, Běláková, Sylvie, and Nováková, Lucie
- Subjects
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SUPERCRITICAL fluid chromatography , *MASS spectrometry , *VITAMIN E , *TOCOTRIENOL , *SERUM , *LIQUID-liquid extraction - Abstract
The goal of this study was to develop an effective supercritical fluid chromatography method using single quadrupole MS for analysis of all isomeric forms of vitamin E. Finally, two fast and effective methods, the high resolution one and the high speed one, for the determination of 8 vitamin E isomers in human serum were developed. Rapid high-throughput liquid-liquid extraction was selected as a sample preparation step. Sample pretreatment of 100 μL human serum was consisted of protein precipitation with 200 μL ethanol and liquid-liquid extraction by 400 μL hexane/dichloromethane (80/20, v/v). The separation was performed on BEH 2-EP (3.0 × 100 mm, 1.7 μm) stationary phase, using isocratic elution with carbon dioxide and 10 mM ammonium formate in methanol in the ratio 98:2 for high resolution method with run time 4.5 min and in the ratio 95:5 for high speed method, where the run time was 2.5 min. The method development included optimization of key parameters: the choice of the suitable stationary phase and the composition of mobile phase, where an influence of various modifiers, their ratio and additives were tested, and optimization of fine tunning parameters including BPR pressure, flow-rate and column temperature. Quantification of all isomeric forms was performed using SIM (single ion monitoring) experiments in ESI positive ion mode. Both high speed and high resolution chromatographic methods were validated in terms of precision, accuracy, range, linearity, LOD, LOQ and matrix effects using the same LLE procedure. The high resolution method provided more sensitive results (LOD: 0.017–0.083 μg mL −1 ) and better linearity (r 2 > 0.9930) than the high speed one (LOD: 0.083–0.25 μg mL −1 , r 2 > 0.9877) at the cost of double time of analysis. [ABSTRACT FROM AUTHOR]
- Published
- 2016
- Full Text
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22. AN LC- MS/MS METHOD FOR THE DETERMINATION OF OMEPRAZOLE ON PROTON PUMP INHIBITOR IN HUMAN PLASMA.
- Author
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Sudha, T., Reddy, V. Kalan Kumar, Hemalatha, P. V., and Ravikumar, V. R.
- Subjects
PROTON pump inhibitors ,OMEPRAZOLE ,LIQUID chromatography-mass spectrometry ,LANSOPRAZOLE ,AMMONIUM acetate ,ACETONITRILE ,MOBILE phase (Chromatography) ,AMMONIUM bicarbonate ,THERAPEUTICS - Abstract
A sensitive and selective liquid chromatographic method coupled with tandem mass spectroscopy (LC-MS/MS) was developed for the quantification of omeprazole in human plasma. Lansoprazole was used as internal standard with plasma samples, extracted using 10mM ammonium acetate. A centrifuged upper layer was then evaporated and reconstituted with Acetonitrile: mobile phase buffer 70:30%v/v. The reconstructed samples were injected into a C18 column purospher star 5µ. The mobile phase was composed of ACN: mobile phase buffer (5mm ammonium bicarbonate buffer) in the ratio of 70:30%v/v with flow rate 1.0mL/min. The mass spectrometer was operated using positive ion mode and turbo electro spray ionisation. Nitrogen was used as the nebulizer, curtain, collision and auxiliary gases. Using MS/MS with multiple reactions monitoring (MRM) mode, omeprazole was detected without severe interferences from plasma matrix. Detection of omeprazole in human plasma was accurate and precision. This method has been successfully applied to the study of omeprazole in human specimens. [ABSTRACT FROM AUTHOR]
- Published
- 2016
- Full Text
- View/download PDF
23. Optimization of Sample Preparation for 1-Hydroxypyrene as a Major Biomarker of Exposure to Polycyclic Aromatic Hydrocarbons Prior to High Performance Liquid Chromatography
- Author
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SJ Shahtaheri, L Ibrahimi, F Golbabaei, M Hosseini, and B Fouladi
- Subjects
Liquid liquid extraction ,1-Hydroxypyrene ,PAHs ,Public aspects of medicine ,RA1-1270 - Abstract
Urinary 1-hydroxypuren (1-OHP) is commonly used as a major metabolite and biological indicator of the overall exposure to polycyclic aromatic hydrocarbons (PAHs). For evaluation of human exposure to such compounds, biological monitoring is an essential process, in which, preparation of samples is one of the most time-consuming and error-prone aspects prior to chromatographic techniques. In this study, non classic form of liquid-liquid extraction (LLE) was optimized with regard to solvent type, solvent volume, extraction temperature, mixing type, and mixing duration. Through the extraction process, a mild temperature was used to keep the compound of interest as stable as possible. In this study, a high performance liquid chromatography, using reverse-phase column was used. The isocratic run was done at a constant flow rate of 0.8 ml/min, the mobile phase was methanol/water and a fluorescence detector was used, setting at 242 nm and 388 nm. At the developed conditions, the extraction recovery was exceeded 87.3%, achieving detection limit of 0.2 µg/l. The factors were evaluated statically and the procedure was validated with three different pools of spiked urine samples and showed a good reproducibility over six consecutive days as well as experiments. It was concluded that, this optimized method could simplify sample preparation for trace residue analysis of PAHs metabolites.
- Published
- 2006
24. Development of salting-out extraction methodology for the determination of piroxicam from polymeric based nanocarriers and biological samples.
- Author
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Tok, Kenan Can, Gumustas, Mehmet, Sengel-Turk, Ceyda Tuba, Amasya, Gulin, Bayram, Bilge, and Arioglu-Inan, Ebru
- Subjects
- *
NANOCARRIERS , *POLYMERIC drug delivery systems , *PIROXICAM , *LUNGS , *ORGANS (Anatomy) , *DRUG delivery systems , *LIQUID-liquid extraction , *DRUGS - Abstract
The aim of the present study is to develop the polymeric nanoparticulate drug delivery systems of piroxicam and to evaluate the in-vitro characteristics such as entrapment efficiency, surface morphology, in-vitro drug release performance, etc. For this reason, a novel HPLC methodology was developed for the determination of piroxicam from its bulk form, pharmaceutical preparation, and nanoparticulate delivery systems. Furthermore, the developed formulation was applied to the rats and the biological samples (plasma, liver, heart, spleen, kidney, and lung homogenates) were analyzed by the developed HPLC method following a salting-out assisted liquid-liquid extraction strategy for the first time in the literature. A Kinetex C18 analytical column (150 mm × 4.6 mm i.d., 5 µm) was used as a stationary phase with a 0.8 mL/min flow rate of acetonitrile: phosphate buffer (40:60, v/v), the column oven was adjusted to 40 °C and detection wavelength is set to 360 nm. Developed method were validated as per selectivity, linearity, LOD, LOQ, precision, and accuracy specified in the International Council for Harmonisation guidelines. As a result of the present study, it has been shown that the analysis of piroxicam from the bulk form, pharmaceutical preparation, developed polymeric-based drug delivery system, and biological samples can be successfully performed and no interferences were observed in any matrix. The developed method was also successfully utilized to study the tissue distribution of piroxicam in rats. [Display omitted] • Piroxicam encapsulated PLGA based nano-sized drug delivery system was developed and characterized. • The in vitro release profiles of PRX from the various PLGA based nanoparticles and the pure API are compared. • Salting out assisted liquid-liquid extraction procedure developed for the first time for PRX analysis. • In vivo distribution of the PRX was demonstrated by animal models. • Green, fast, and sensitive HPLC method was developed for the determination and validation of PRX in plasma and tissues. [ABSTRACT FROM AUTHOR]
- Published
- 2022
- Full Text
- View/download PDF
25. Approche expérimentale et théorique pour l'étude de l'extraction de l'acide nitrique et de certains produits de fission
- Author
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Dru, Valentin, Institut de Chimie Séparative de Marcoule (ICSM - UMR 5257), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Université Montpellier, Jean-François Dufrêche, STAR, ABES, and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)
- Subjects
[CHIM.OTHE] Chemical Sciences/Other ,Modélisation ,Speciation ,Liquid liquid extraction ,Extraction liquide liquide ,Spéciation ,[CHIM.OTHE]Chemical Sciences/Other ,Modelling - Abstract
Solvent extraction models as the ones developed by the CEA required a precise description of extraction equilibria taking into account explicitely the deviation from ideality and the speciation of the different elements involved. Firstly, binary data acquisition of ruthenium nitrosylnitrate, problematic electrolyte in the Purex process, for the determination of the deviation from ideality has been performed for water activity between 1 and 0.750. The chemical properties of this electrolyte required the development of new methodologies to adapt the simple solution approach to mixtures exhibiting a deviation from this behavior. Secondly, nitric acid speciation in the organic phase, required to determine the quantity of free TBP in solution, has been studied throught the analysis of experimental data two different systems : TBP/HNO3/H2O/TPH and TBP/HNO3. The highlighting of the importance of water for the formation of clusters observed experimentally allows the proposition of a model depending on the concentration of nitric acid in the organic phase., Les modèles d’extraction liquide-liquide comme ceux développés par le CEA nécessitent une description précise des équilibres d’extraction prenant en compte explicitement les écarts à l’idéalité ainsi que la spéciation des différents éléments en présence. Dans un premier temps, l’acquisition des données binaires du nitrate de ruthénium nitrosyle, électrolyte posant problème dans le procédé Purex, pour la détermination des écarts à l’idéalité a été réalisée pour une gamme d’activité d’eau allant de 1 à 0,750. Les propriétés chimiques de cet électrolyte ont demandé le développement de nouvelles méthodologies pour adapter l’approche des solutions simples aux mélanges présentant un écart à ce comportement. Dans un second temps, la spéciation de l’acide nitrique en phase organique, nécessaire à la détermination de la quantité de TBP libre en solution, a été étudié via l’analyse de résultats expérimentaux issus des systèmes TBP/HNO3/H2O/TPH et TBP/HNO3. La mise en évidence du rôle de l’eau dans la formation des clusters observés expérimentalement a permis de proposer un modèle en fonction de la concentration d’acide nitrique en phase organique.
- Published
- 2020
26. Validation of an Analytical Method for Simultaneous Determination of 18 Persistent Organic Pollutants in Trout Using LLE Extraction and GC-MS/MS
- Author
-
Bayat, Mitra, tehrani, Mohammad Saber, Kobarfard, Farzad, Husain, Syed Waqif, and Yazdanpanah, Hassan
- Subjects
Polychlonitated biphenyls ,Trout ,GC-MS/MS ,Persistent Organic Pollutant (POPs) ,Organochlorine pesticides ,Original Article ,Iran ,Liquid Liquid Extraction - Abstract
Persistent organic pollutants, (POPs), are vast distributed compounds in environment which are recognized as one of the global pollution problems. These groups of materials being dangerous due to their high stability are accumulated in animal tissues and occurring in the food chain. One of the major paths through which persistent organic combinations access to human body is consuming polluted foods, particularly, fishes. Among aquatic animals, trout as one of the mostly consumed fishes in Tehran’s food basket was studied. In this study, two categories of persistent organic pollutants: Organochlorine pesticides (OCPs) including HCB, Dieldrin, Methoxychlor, α-, ϒ-Chlordane, α-, β-Endosulfan and o,p’-DDE, p,p’-DDE, o,p’-DDT, p,p’-DDT and the second group Polychlonitated biphenyls (PCBs) including seven PCB congeners which are called indicator PCBs (IUPAC nos.: 28,52,101,118,138,153 and 180) were determined in trout by GC-MS/MS in MRM monitoring mode and LLE extraction. The average recoveries of OCPs and PCBs at five concentration levels (1, 2, 5, 10 and 20 ng/g for PCBs and 5 times for OCPs) were in the range of 73-112%. The relative standard deviations of POPs in fish were in the range of 1.4-17.9% for all of the concentration levels. The limit of detections (LODs) and the limit of quantitations (LOQs) were between 0.6-8.3 and 2-25 µg/kg, respectively. The results indicated the presence of organochlorine pesticides in trout and the levels of p,p’-DDE and p,p’-DDT were within the range of < LOQ -12.83 and < LOQ -10.2 ng/g ww (wet weight), respectively. According to the results, OCPs residues were lower than maximum residue levels set by European Council Directives.
- Published
- 2020
27. Separation techniques in butanol production: Challenges and developments.
- Author
-
Abdehagh, Niloofar, Tezel, F. Handan, and Thibault, Jules
- Subjects
- *
BUTANOL , *SEPARATION (Technology) , *PETROLEUM , *NATURAL resources , *POLITICAL stability , *BIODIESEL fuels , *ETHANOL as fuel , *RENEWABLE energy sources , *ECONOMICS - Abstract
Abstract: The rising cost of crude oil combined with the depletion of the resources, political instability in oil producing countries, and the desire to reduce the current dependence on imported oil are some of the reasons that have motivated the different waves of interest for renewable and sustainable fuels. In addition to bioethanol and biodiesel, biobutanol is attracting significant interest as a biofuel mainly due to the recent advances in biotechnology for its production. Biobutanol has lower water miscibility, flammability, and corrosiveness than ethanol, and has the enviable advantage to be able to directly replace gasoline in car engines without requiring modifications. Butanol can be produced from a wide variety of waste biomass feedstock which does not compete with food. In butanol bioproduction, the most widely used microorganisms for acetonebutanol–ethanol (ABE) fermentation are anaerobic bacteria such as the solventogenic Clostridia including Clostridium acetobutylicum and Clostridium beijerinckii. However, the production of biobutanol via fermentation is facing significant engineering challenges due to the very low final concentration and low yield due to the severe butanol toxicity to microorganisms. It is therefore important to find an efficient separation technique to recover butanol at the end of fermentation or during the fermentation to reduce the level of toxicity and prolong the fermentation. In this article, the main butanol separation techniques such as adsorption, gas stripping, liquid–liquid extraction (LLE), perstraction, reverse osmosis (RO) and pervaporation were discussed. It was concluded that adsorption and pervaporation are the separation techniques that offer the most potential for butanol separation from dilute solutions. [Copyright &y& Elsevier]
- Published
- 2014
- Full Text
- View/download PDF
28. Ionic liquid-based liquid phase microextraction with direct injection for capillary electrophoresis
- Author
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Breadmore, Michael C.
- Subjects
- *
EXTRACTION (Chemistry) , *CAPILLARY electrophoresis , *IONIC liquids , *CLOZAPINE , *METABOLITES , *DRUG monitoring , *FORENSIC toxicology , *MICROCHEMISTRY - Abstract
Abstract: Liquid–liquid microextraction using the water immiscible ionic liquid, 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, EMIM NtfO2, for the concentration and cleanup of basic compounds for analysis by CE has been investigated. Using an electrolyte comprising 1mol/L alanine and 3mol/L acetic acid, EMIM NtfO2 could be directly injected into the capillary after liquid phase extraction. Using the basic dye chryisoidine, sensitivity enhancements approaching 1000-fold were obtained by mixing 20μL of EMIM NtfO2 with 1500μL of aqueous sample, leaving only 5μL of the undissolved ionic liquid which was used for injection into the CE. Lower more repeatable enhancement factors of 200-fold were obtained with slightly larger initial 25μL volumes of EMIM NtfO2 due to the larger residual volume of ionic liquid which made handling easier. This could be extended to basic pharmaceuticals, and the extraction of clozapine and its two active metabolites, nor-clozapine and clozapine-N-oxide, was demonstrated from urine with enrichment factors greater than 100 obtained. Handling of potentially more dangerous samples, such as serum, through in-vial extraction of clozapine and its metabolites and direct injection of the ionic liquid layer was also demonstrated with enhancements in sensitivity of 80. Limits of detection from 3 to 11μg/L and 6 to 55μg/L were obtained from urine and serum, respectively, which are sufficiently low to be useful for the determination of these pharmaceuticals clinically for therapeutic drug monitoring and for forensic toxicology. [Copyright &y& Elsevier]
- Published
- 2011
- Full Text
- View/download PDF
29. Serum metabolite profiling of ST-segment elevation myocardial infarction using liquid chromatography quadrupole time-of-flight mass spectrometry
- Author
-
Fatma Demirkaya Miloglu, A. M. Abd El-Aty, Gulsah Gundogdu, Fuat Gundogdu, Ahmet Hacimuftuoglu, Onur Senol, and Yavuzer Koza
- Subjects
Male ,propionic acid ,Metabolite ,Clinical Biochemistry ,isoleucine ,arginine ,030226 pharmacology & pharmacy ,01 natural sciences ,Biochemistry ,Mass Spectrometry ,Analytical Chemistry ,low density lipoprotein cholesterol ,Palmitic acid ,chemistry.chemical_compound ,0302 clinical medicine ,Fumarates ,LC/Q-TOF/MS/MS ,high density lipoprotein cholesterol ,valine ,Drug Discovery ,middle aged ,palmitic acid ,succinic acid ,hyperlipidemia ,betaine ,proline ,Amino Acids ,caffeine ,malonic acid ,clinical article ,C reactive protein ,adult ,liquid liquid extraction ,General Medicine ,Middle Aged ,time of flight mass spectrometry ,metabolomics ,female ,diabetes mellitus ,Metabolome ,Female ,Leucine ,alanine ,leucine ,leukocyte ,cardiovascular risk ,Fumaric acid ,hypertension ,Maleic acid ,maleic acid ,glycerol ,urea ,Malonic acid ,Article ,smoking ,STEMI ,serine ,03 medical and health sciences ,determination ,male ,liquid chromatography ,Humans ,Metabolomics ,controlled study ,fumaric acid ,human ,Molecular Biology ,Pharmacology ,metabolic fingerprinting ,Chromatography ,lysine ,ST segment elevation myocardial infarction ,010401 analytical chemistry ,quadrupole mass spectrometry ,carnitine ,lactic acid ,Maleates ,citric acid ,threonine ,body mass ,Malonates ,0104 chemical sciences ,triethanolamine ,Oleic acid ,chemistry ,oleic acid ,phosphatidylethanolamine ,ST Elevation Myocardial Infarction ,Amino Acids/blood ,Chromatography, Liquid/*methods ,Fumarates/blood ,Maleates/blood ,Malonates/blood ,Mass Spectrometry/*methods ,Metabolome/physiology ,Metabolomics/*methods ,ST Elevation Myocardial Infarction/blood/metabolism ,Isoleucine ,butyric acid ,glycine ,Chromatography, Liquid - Abstract
ST segment elevation myocardial infarction (STEMI) is one of the most common global causes of cardiovascular disease-related death. Several metabolites may change during STEMI. Hence, analysis of metabolites in body fluid may be considered as a rapid and accurate test for initial diagnosis. This study has therefore attempted to determine the variation in metabolites identified in the serum of STEMI patients (n = 20) and 15 controls. Samples collected from the Cardiology Department, Medical Faculty, Ataturk University, were extracted by liquid–liquid extraction and analysed using liquid chromatography quadrupole time-of-flight mass spectrometry. The METLIN database was used for the identification and characterization of metabolites. According to Q-TOF/MS measurements, 231 m/z values, which were significantly different between groups (P < 0.01 and fold analysis >1.5) were detected. Metabolite identification was achieved via the Human Metabolome database. According to the multivariate data analysis, leucine, isoleucine, l-proline, l-alanine, glycine, fumaric acid, citrate, succinate and carnitine levels were decreased, whereas levels of propionic acid, maleic acid, butyric acid, urea, oleic acid, palmitic acid, lysoPC [18:2(9Z)], glycerol, phoshpatidylethanolamine, caffeine and l-lactic acid were increased in STEMI patients compared with controls. In conclusion, malonic acid, maleic acid, fumaric acid and palmitic acid can be used as biomarkers for early risk stratification of patients with STEMI. © 2019 John Wiley & Sons, Ltd.
- Published
- 2020
30. AN LC- MS/MS METHOD FOR THE DETERMINATION OF OMEPRAZOLE ON PROTON PUMP INHIBITOR IN HUMAN PLASMA
- Author
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Kalan Kumar Reddy, P. V. Hemalatha, V. R. Ravikumar, and T. Sudha
- Subjects
Lansoprazole ,Analytical chemistry ,Pharmaceutical Science ,lcsh:RS1-441 ,Pharmacy ,Proton pump inhibitor ,Mass spectrometry ,01 natural sciences ,omeprazole ,Matrix (chemical analysis) ,lcsh:Pharmacy and materia medica ,chemistry.chemical_compound ,medicine ,Pharmacology (medical) ,LC-MS/MS ,Acetonitrile ,Omeprazole ,Chromatography ,010405 organic chemistry ,010401 analytical chemistry ,Extraction (chemistry) ,liquid liquid extraction ,lansoprazole ,0104 chemical sciences ,Ammonium bicarbonate ,chemistry ,Ammonium acetate ,medicine.drug - Abstract
A sensitive and selective liquid chromatographic method coupled with tandem mass spectroscopy (LC-MS/MS) was developed for the quantification of omeprazole in human plasma. Lansoprazole was used as internal standard with plasma samples, extracted using 10mM ammonium acetate. A centrifuged upper layer was then evaporated and reconstituted with Acetonitrile: mobile phase buffer 70:30%v/v. The reconstructed samples were injected into a C 18 column purospher star 5µ. The mobile phase was composed of ACN: mobile phase buffer (5mm ammonium bicarbonate buffer) in the ratio of 70:30%v/v with flow rate 1.0mL/min. The mass spectrometer was operated using positive ion mode and turbo electro spray ionisation. Nitrogen was used as the nebulizer, curtain, collision and auxiliary gases. Using MS/MS with multiple reactions monitoring (MRM) mode, omeprazole was detected without severe interferences from plasma matrix. Detection of omeprazole in human plasma was accurate and precision. This method has been successfully applied to the study of omeprazole in human specimens Keywords: Proton pump inhibitor, omeprazole, lansoprazole, LC-MS/MS, liquid liquid extraction
- Published
- 2016
31. Recent sample pretreatment methods for determination of selective serotonin reuptake inhibitors (SSRIs) in biological samples.
- Author
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Chen, Li, Wang, Jincheng, Xu, Tyllis, Feng, Xinrui, Huang, Chuixiu, and Shen, Xiantao
- Subjects
- *
SEROTONIN uptake inhibitors , *ANTIDEPRESSANTS , *SOLID phase extraction , *SAMPLING methods , *EXTRACTION techniques - Abstract
• Sample preparation methods for SSRI analysis in biological samples are important. • Traditional LLE and SPE in SSRI analysis are summarized. • Miniaturized extraction methods (SPME, LPME and EME) in SSRI analysis are reviewed. • Prospects of sample pretreatment methods for SSRI analysis are presented. [Display omitted] Selective serotonin reuptake inhibitors (SSRIs) such as fluoxetine (FLU), sertraline (SER), paroxetine (PAR), fluvoxamine (FLV) and citalopram (CIT) have been the first treatment drugs for pregnant and breastfeeding women. Quantitative analysis of SSRIs in biological samples is extremely needed in public health and clinical practice. During the analysis, sample pretreatment is an important step that can obtain an accurate quantitative analysis of SSRIs in the complex samples. The present paper discussed the recent development of sample preparation methods for SSRI analysis. Traditional sample preparation techniques such as liquid liquid extraction (LLE) and solid phase extraction (SPE), which have been widely used in the separation of SSRIs in biological samples, were extensively presented. Moreover, the new sample preparation techniques including liquid phase microextraction (LPME), solid phase microextraction (SPME), electromembrane extraction (EME) and other miniaturized extraction techniques, which are becoming highly popular in SSRI analysis, were also critically reviewed. In this review, both the advantages and disadvantages of these sample pretreatment methods were addressed. As a summary, we prospected the challenges and promising directions for the future of sample pretreatment methods in SSRI analysis. [ABSTRACT FROM AUTHOR]
- Published
- 2021
- Full Text
- View/download PDF
32. Determination and pharmacokinetics of dextromoramide in methadone maintenance therapy.
- Author
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Ufkes, J.G.R., de Vos, J.W., and van Brussel, G.H.A.
- Abstract
To study the pharmacokinetics of dextromoramide in long term opiate addicts on methadone maintenance therapy (MMT) a reverse phase HPLC technique was developed to monitor dextromoramide and methadone concentrations in plasma simultaneously. After liquid liquid extraction from plasma, dextromoramide and methadone were determined using a Supelcosil LC ABZ column and a mobile phase of KH2phosphate buffer (25 mM, pH 2.5) mixed with acetonitrile (80:20, v/v) and UV detection at 206 nm. The method was found to be sufficiently sensitive, specific and reproducible to apply in six subjects on MMT for many years, receiving orally administered dextromoramide as adjuvant. Pharmacokinetic data sets for dextromoramide in each subject were conducted and analysed further, indicating short elimination half life values (71 min, range 31 152 min). Contrary to previous studies, in all subjects tested the pharmacokinetics of dextromoramide are best described using an one compartment model. [ABSTRACT FROM AUTHOR]
- Published
- 1998
- Full Text
- View/download PDF
33. Lampante olive oil refining with supercritical carbon dioxide.
- Author
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Bondioli, P., Mariani, C., Lanzani, A., Fedeli, E., Mossa, A., and Muller, A.
- Abstract
Lampante olive oil has been treated in a supercritical CO extraction plant operating in a continuous countercurrent mode. We report the results of a systematic investigation to define the optimal operative parameters. We also have examined the compositional variation of lampante olive oil samples with different characteristics and of different geographic origins before and after refining at optimal conditions. Although practical feasibility of the proposed procedure can be questioned, the results demonstrate the possibility of fractionating components contained in the starting oil even if present at trace levels. [ABSTRACT FROM AUTHOR]
- Published
- 1992
- Full Text
- View/download PDF
34. Sample preparation for photometric determination of histamine in foodstuffs compared with capillary electrophoresis.
- Author
-
Mahendradatta, Meta and Schwedt, G.
- Abstract
To determine levels of histamine, two methods were used, photometry in conjunction with two sample clean-up procedures, and capillary zone electrophoresis (CZE). The two sample clean-up procedures used were liquid liquid extraction (LLE) with n-butanol and solid phase extraction (SPE). Using CZE, the separation of histamine from the matrix was good. The other method, photometry, represents a classic and simple method, that can be employed for in situ measurement of histamine. We found that it was necessary to clean up the samples prior to photometry; if this was not done, the recorded levels of histamine were higher than those determined by CZE. In order to determine levels of histamine, both of these rapid tests were applied to ten different foodstuffs. The levels of histamine measured using photometry following either LLE or SPE were compared. The results indicated that photometry is a suitable method for the measurement of histamine, although the sample solutions have to be purified by either LLE or SPE. Samples do not need to be cleaned up before CZE because there is no interference between histamine and attendant material. Both sample clean-up procedures were applied to the following foodstuffs: tomatoes, sauerkraut, tuna, leaf spinach, cream spinach, white wine and mackerel. The differences of the measured values vary between 3% and 18% for LLE and 6% and 27% for SPE. For the other foodstuffs, such as beef, beer and non-alcoholic beer, only one sample clean-up procedure is suitable. LLE used for beef and beer leads to differences in measured levels of histamine between 18% and 50%, respectively, whereas SPE used for non-alcoholic beer leads to differences of 20%. [ABSTRACT FROM AUTHOR]
- Published
- 1998
- Full Text
- View/download PDF
35. Gloeothece sp. as a Nutraceutical Source—An Improved Method of Extraction of Carotenoids and Fatty Acids
- Author
-
Helena M. Amaro, Marco Preto, F. Xavier Malcata, Isabel Sousa-Pinto, A. Catarina Guedes, Faculdade de Engenharia, and CIIMAR - Centro Interdisciplinar de Investigação Marinha e Ambiental
- Subjects
0106 biological sciences ,Green chemistry ,Antioxidant ,antioxidant ,medicine.medical_treatment ,Pharmaceutical Science ,01 natural sciences ,cyanobacteria ,Antioxidants ,Drug Discovery ,pressurized liquid extraction ,Microalgae ,Biomass ,lcsh:QH301-705.5 ,Pharmacology, Toxicology and Pharmaceutics (miscellaneous) ,Carotenoid ,comparative study ,ABTS radical scavenging assay ,chemistry.chemical_classification ,beta carotene ,alcohol ,ultrasound ,Chemistry ,Fatty Acids ,Temperature ,liquid liquid extraction ,polyunsaturated fatty acid ,carotenoid ,solvent extraction ,Solvent ,Ultrasonic Waves ,validation study ,nutraceutical ,flow rate ,biological product ,chemical parameters ,Gloeothece ,Liquid-Liquid Extraction ,chemistry ,Cyanobacteria ,environmental impact ,Article ,Nutraceutical ,process optimization ,cyanobacterium ,Liquid–liquid extraction ,010608 biotechnology ,biomass production ,medicine ,chemical composition ,controlled study ,procedures ,intermethod comparison ,temperature dependence ,continuous pressurized solvent extraction ,Biological Products ,nonhuman ,solvent effect ,ultrasound assisted extraction ,Chromatography ,Ethanol ,green chemistry ,isolation and purification ,solvent volume ,010401 analytical chemistry ,Green Chemistry Technology ,economics ,antioxidant assay ,Biological product ,Carotenoids ,microalga ,0104 chemical sciences ,lcsh:Biology (General) ,dietary supplement ,Dietary Supplements ,DPPH radical scavenging assay ,CPSE ,fatty acid ,Solvent effects ,PUFA - Abstract
The nutraceutical potential of microalgae boomed with the exploitation of new species and sustainable extraction systems of bioactive compounds. Thus, a laboratory-made continuous pressurized solvent extraction system (CPSE) was built to optimize the extraction of antioxidant compounds, such as carotenoids and PUFA, from a scarcely studied prokaryotic microalga, Gloeothece sp. Following &ldquo, green chemical principles&rdquo, and using a GRAS solvent (ethanol), biomass amount, solvent flow-rate/pressure, temperature and solvent volume&mdash, including solvent recirculation&mdash, were sequentially optimized, with the carotenoids and PUFA content and antioxidant capacity being the objective functions. Gloeothece sp. bioactive compounds were best extracted at 60 °, C and 180 bar. Recirculation of solvent in several cycles (C) led to an 11-fold extraction increase of &beta, carotene (3C) and 7.4-fold extraction of C18:2 n6 t (5C) when compared to operation in open systems. To fully validate results CPSE, this system was compared to a conventional extraction method, ultrasound assisted extraction (UAE). CPSE proved superior in extraction yield, increasing total carotenoids extraction up 3-fold and total PUFA extraction by ca. 1.5-fold, with particular extraction increase of 18:3 n3 by 9.6-fold. Thus, CPSE proved to be an efficient and greener extraction method to obtain bioactive extract from Gloeothece sp. for nutraceutical purposes&mdash, with low levels of resources spent, while lowering costs of production and environmental impacts.
- Published
- 2018
36. Separation of 206Po from alpha particle irradiated lead bismuth eutectic target.
- Author
-
Naskar, Nabanita and Lahiri, Susanta
- Subjects
- *
ALPHA rays , *CYCLOTRONS , *BISMUTH , *RADIOISOTOPES , *POLONIUM , *TRIOCTYLAMINE - Abstract
Lead bismuth eutectic (LBE) target was bombarded with 46 MeV α-particle. Possibility of separation of no-carrier-added (NCA) polonium radioisotopes from the bulk lead-bismuth eutectic target was explored. Differential precipitation showed presence of Po with bulk Bi, leaving behind bulk Pb in aqueous medium. NCA 206Po radioisotope was then separated from bulk Bi using trioctylamine (TOA) as the extractant. At best condition of 0.01 M TOA+0.1 M HCl, highest separation factor (>500) was achieved between NCA Po and bulk Bi. • Cyclotron production of Po radioisotopes from alpha-irradiated LBE target. • Differential precipitation separated bulk Pb from bulk Bi and Po. • Radiochemical separation of 206Po from bulk Bi using anion exchanger. • Applicable for decontaminating long-lived, alpha-emitting Po from LBE. • First radiochemical attempt to separate Po from LBE sequentially. [ABSTRACT FROM AUTHOR]
- Published
- 2021
- Full Text
- View/download PDF
37. Extraction of medium chain fatty acids from organic municipal waste and subsequent production of bio-based fuels
- Author
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Johannes Jager, Jan Kannengiesser, Liselotte Schebek, Kaori Sakaguchi-Söder, Timo Mrukwia, and Publica
- Subjects
anaerobic digestion ,biobased fuels ,procedure ,waste technology ,organic municipal waste ,elongation ,02 engineering and technology ,010501 environmental sciences ,01 natural sciences ,bioreactor ,percolation ,chemistry.chemical_compound ,valeric acid ,Waste Management ,Germany ,energy metabolism ,octanoic acid ,0202 electrical engineering, electronic engineering, information engineering ,Organic chemistry ,biofuel production ,Waste Management and Disposal ,chemistry.chemical_classification ,Hexanoic acid ,Biodiesel ,alcohol ,Hydrolysis ,refining ,saturated fatty acid ,Chains ,liquid liquid extraction ,municipal solid waste ,Clostridium kluyveri ,Waste treatment ,acetic acid ,degradation kinetics ,priority journal ,greenhouse gas ,medium chain fatty acid ,biofuel ,percolation (solid state) ,fuel ,volatile fatty acid ,waste treatment ,devices ,bbutyric acid ,020209 energy ,extraction method ,fuel additive ,biodiesel ,process control ,Raw material ,volatile ,oils and fats ,Biogas ,chemical composition ,controlled study ,waste ,liquid ,anaerobic treatments ,0105 earth and related environmental sciences ,bio-based fuel ,nonhuman ,Chromatography ,concentration (parameters) ,carbon ,Fatty acid ,fatty acid analysis ,Fatty Acids, Volatile ,fermentation process ,chain elongation ,solvents ,chemistry ,Biofuels ,viscosity ,Fermentation ,composting ,extraction ,fatty acid ,hexanoic acid ,metabolism ,waste treatment process - Abstract
This paper provides an overview on investigations for a new technology to generate bio-based fuel additives from bio-waste. The investigations are taking place at the composting plant in Darmstadt-Kranichstein (Germany). The aim is to explore the potential of bio-waste as feedstock in producing different bio-based products (or bio-based fuels). For this investigation, a facultative anaerobic process is to be integrated into the normal aerobic waste treatment process for composting. The bio-waste is to be treated in four steps to produce biofuels. The first step is the facultative anaerobic treatment of the waste in a rotting box namely percolate to generate a fatty-acid rich liquid fraction. The Hydrolysis takes place in the rotting box during the waste treatment. The organic compounds are then dissolved and transferred into the waste liquid phase. Browne et al. (2013) describes the hydrolysis as an enzymatically degradation of high solid substrates to soluble products which are further degraded to volatile fatty acids (VFA). This is confirmed by analytical tests done on the liquid fraction. After the percolation, volatile and medium chain fatty acids are found in the liquid phase. Concentrations of fatty acids between 8.0 and 31.5 were detected depending on the nature of the input material. In the second step, a fermentation process will be initiated to produce additional fatty acids. Existing microorganism mass is activated to degrade the organic components that are still remaining in the percolate. After fermentation the quantity of fatty acids in four investigated reactors increased 3-5 times. While fermentation mainly non-polar fatty acids (pentanoic to octanoic acid) are build. Next to the fermentation process, a chain-elongation step is arranged by adding ethanol to the fatty acid rich percolate. While these investigations a chain-elongation of mainly fatty acids with pair numbers of carbon atoms (acetate, butanoic and hexanoic acid) are demonstrated. After these three pre-treatments, the percolate is brought to a refinery to extract the non-polar fatty acids using bio-diesel, which was generated from used kitchen oil at the refinery. The extraction tests in the lab have proved that the efficiency of the liquid-liquid-extraction is directly linked with the chain length and polarity of the fatty acids. By using a non-polar bio-diesel mainly the non-polar fatty acids, like pentanoic to octanoic acid, are extracted. After extraction, the bio-diesel enriched with the fatty acids is esterified. As a result bio-diesel with a lower viscosity than usual is produced. The fatty acids remaining in the percolate after the extraction can be used in another fermentation process to generate biogas.
- Published
- 2016
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38. Enhanced Chromatographic Determination of Nicotine in Human Plasma: Applied to Human Volunteers
- Author
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Ayoub, Bassam M., Mohamady, Samy, Hendy, Moataz S., and Elmazar, Mohamed M.
- Subjects
human volunteers ,Nicotine ,vacuum evaporation ,UPLC ,human plasma ,Liquid liquid extraction ,Original Article - Abstract
Development of enhanced UPLC-UV method for determination of nicotine in human plasma was achieved on a Symmetry(®) C18 column (100 mm × 2.1 mm, 2.2 μm) applying isocratic elution based on Methanol: Acetonitrile: Phosphate Buffer (pH: 2.7) with the ratio (20:30:50, v/v/v) as a mobile phase. The ultraviolet detector was operated at 260 nm. The mobile phase was pumped through the column at a flow rate of 0.2 mL min(-1). The column temperature was adjusted to 50ºC and the injection volume was 2 μL. Quinine was selected as an internal standard (IS) due to its structure similarity to nicotine having basic pyridine ring to optimize the liquid liquid extraction procedure using diethyl ether coupled with vacuum evaporation at 40°C. Validation parameters for nicotine were found to be acceptable over the concentration range of 2.5-50 ng ml(-1). The application of the proposed method on four healthy human volunteers was approved by the ethical committee. The study was carried out under fasting conditions and the concerned subjects were informed about the objectives and possible risks involved in the study. The proposed method proved to be simple and fast which is a major advantage to analyze large number of samples per day using the accelerated vacuum evaporation technique. The method showed satisfactory data for all the parameters tested within the limits for bioanalytical assays. The lower limit of quantification (LLOQ) permits the application of the method for further pharmacological and clinical studies.
- Published
- 2015
39. Sample preparation: A critical step in the analysis of cholesterol oxidation products
- Author
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Georgiou, Christiana A., Constantinou, Michalis S., Kapnissi‐Christodoulou, Constantina P., and Kapnissi‐Christodoulou, Constantina P. [0000-0003-3755-1052]
- Subjects
lipid analysis ,gas chromatography ,Cholesterol oxidation products ,dissolution ,acylglycerol ,Extraction ,propanol ,Analytical method ,Sample preparation procedure ,Analytical Chemistry ,high temperature ,Cholesterol, Dietary ,Human health ,Lipid extraction ,Sample preparation ,Solid phase extraction ,Process engineering ,Ketocholesterols ,degradation ,emulsion ,milk ,Saponification ,chloroform ,Chemistry ,Hydrolysis ,Solid Phase Extraction ,vitamin ,liquid liquid extraction ,General Medicine ,solvent extraction ,unclassified drug ,hexane ,fat intake ,Cholesterol ,cholesterol ester ,triacylglycerol ,room temperature ,Oxidation-Reduction ,high performance liquid chromatography ,purification ,Liquid-Liquid Extraction ,review ,Phase separation ,Food Contamination ,Food safety ,Oxidation ,phospholipid ,methanol ,Solid-phase extraction ,reliability ,Chromatography ,Cholestanes ,business.industry ,Extraction (chemistry) ,Analytic Sample Preparation Methods ,Hydroxycholesterols ,Consumer Product Safety ,Stationary phase ,Epoxy Compounds ,Extraction and purifications ,fatty acid ,diet ,business ,cholesterol oxidation product ,Food Analysis ,Food Science - Abstract
In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity. © 2013 Elsevier Ltd. All rights reserved. 145 918 926 Cited By :11
- Published
- 2014
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40. Thorium determination in aqueous solutions after separation by ion-exchange and liquid extraction
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Kiliari, T., Pashalidis, Ioannis, and Pashalidis, Ioannis [0000-0002-7587-6395]
- Subjects
Health, Toxicology and Mutagenesis ,ultraviolet spectroscopy ,Analytical chemistry ,chemistry.chemical_element ,Cation exchange ,Standard solution ,Physico-chemical parameters ,salinity ,thorium ,Analytical Chemistry ,Metal ,Colloid ,water sampling ,Thorium determination ,physical chemistry ,Radiology, Nuclear Medicine and imaging ,colloid ,Spectroscopy ,separation technique ,Aqueous solution ,quantitative analysis ,Ion exchange ,pH ,actinide ,article ,Public Health, Environmental and Occupational Health ,liquid liquid extraction ,Thorium ,Actinide ,Contamination ,calibration ,Pollution ,Liquid extraction ,Nuclear Energy and Engineering ,chemistry ,visual_art ,visual_art.visual_art_medium ,resin ,aqueous solution ,Chemical recovery - Abstract
The concentration of thorium in aqueous samples has been determined by means of alpha-spectroscopy and UV-Vis photometry after chemical separation and pre-concentration of the actinide by cation exchange and liquid-liquid extraction using Chelex-100 resin and 30%TBP in dodecan, respectively. Method calibration was performed using thorium standard solutions and resulted in a high chemical recovery for cation exchange and liquid extraction. Regarding, the effect of physicochemical parameters (e.g., pH, salinity, competitive cations, and colloidal species) on the separation recovery of thorium from aqueous solutions by cation exchange has also been investigated. The investigation was performed to evaluate the applicability of cation exchange and liquid extraction as separation and pre-concentration methods prior to the quantitative analysis of thorium in water samples, and has shown that the method could be successfully applied to waters with relatively low-salinity and metal ion contamination. © 2011 Akadémiai Kiadó. 288 3 753 758 Cited By :8
- Published
- 2011
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41. Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection
- Author
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Thomas Wenzl, Abdullah Akdogan, and Gerhard Buttinger
- Subjects
Chrysene ,Aromatic compounds ,Chromatography, High Pressure Liquid ,Fluorescence ,Laboratories ,Plant Oils/*chemistry ,Polycyclic Aromatic Hydrocarbons/*analysis ,Solid Phase Extraction ,Spectrometry, Fluorescence ,Health, Toxicology and Mutagenesis ,limit of quantitation ,polycyclic aromatic hydrocarbons ,Aromatic hydrocarbons ,Extraction ,chrysene ,Toxicology ,01 natural sciences ,chemistry.chemical_compound ,Oils and fats ,Concentration levels ,Single laboratory validations ,Sample preparation ,Solid phase extraction ,Polycyclic Aromatic Hydrocarbons ,corn oil ,benzo[b]fluoranthene ,media_common ,Liquid partitioning ,Chromatography ,limit of detection ,Saponification ,Hydrolysis ,Pyrene ,benzo[a]pyrene ,liquid liquid extraction ,04 agricultural and veterinary sciences ,General Medicine ,olive oil ,040401 food science ,Method validations ,vegetable oil ,priority journal ,validation study ,Aromatization ,Uncertainty analysis ,sunflower oil ,fluorescence ,measurement accuracy ,high performance liquid chromatography ,benz[a]anthracene ,Liquid chromatography ,Phase separation ,chemistry ,Article ,0404 agricultural biotechnology ,polycyclic aromatic hydrocarbon ,media_common.cataloged_instance ,Plant Oils ,HPLC-fluorescence detection ,European union ,high-performance liquid chromatography ,sesame seed oil ,Fluoranthene ,Detection limit ,Solid-phase extraction ,010401 analytical chemistry ,Public Health, Environmental and Occupational Health ,Edible oil ,Limits of detection ,spectrofluorometry ,Liquids ,General Chemistry ,Hydrocarbons ,0104 chemical sciences ,Relative measurement ,measurement repeatability ,laboratory ,Food Science - Abstract
An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid–liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg-1. The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg-1 and from 0.13 to 0.24 µg kg-1. Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg-1), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples. © 2016 The Author(s). Published by Taylor & Francis.
- Published
- 2016
42. A multi-residue method for determination of 36 endocrine disrupting chemicals in human serum with a simple extraction procedure in combination of UPLC-MS/MS analysis.
- Author
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Wang, Yun, Li, Guoliang, Zhu, Qingqing, and Liao, Chunyang
- Subjects
- *
ENDOCRINE disruptors , *PHTHALATE esters , *BISPHENOL A , *SOLID phase extraction , *TANDEM mass spectrometry , *MATRIX effect , *SERUM , *TOXICOLOGICAL chemistry - Abstract
Much attention has been paid to endocrine disrupting chemicals (EDCs) due to their widespread presence in various environmental matrices, and endocrine disrupting potential even at low concentrations. However, little is known about the multiple EDCs exposure to human and related adverse effects on health, which warrants a multi-residue method for simultaneous determination of EDCs in human samples such as serum. In this study, we developed and validated a novel method for determination of 36 EDCs (8 bisphenols, 7 parabens, 2 antimicrobials, 5 benzophenones, and 14 phthalate metabolites) in human serum with ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Two extraction methods (liquid liquid extraction (LLE), and LLE coupled with solid phase extraction (SPE) clean-up) were compared, and eleven solvents and two SPE cartridges were optimized for extraction and clean-up procedure, respectively. Recoveries of target compounds spiked in human serum at three levels of concentrations (0.5, 2.5 and 10 ng/mL) ranged from 45.8% to 120%, and the relative standard deviations (RSDs) were lower than 20%. The linearity of the labeled dilution calibration curve was good with correlation coefficient ranging from 0.995 to 0.999, and the limits of quantification (LOQs) were between 0.002 and 0.532 ng/mL. Low RSDs of intra-day (0.1–12.7%) and inter-day (0.2–13.3%) revealed the accuracy and precision of the quantification. The method was successfully applied to determine the target EDCs in human serum samples from 14 randomly selected individuals. The developed method is a promising method for routine measurement of EDCs in human serum. Image 1 • A simple and robust method for simultaneous determination of 36 EDCs in serum by UPLC-MS/MS was developed. • The pretreatment of LLE extraction in combination with SPE clean-up achieved high recovery and low matrix effect. • MeOH/ACN and MCX were optimized as the better extraction solvent and clean-up SPE cartridge, respectively. • The developed method was validated and successfully applied for determination of real human serum. [ABSTRACT FROM AUTHOR]
- Published
- 2019
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- View/download PDF
43. Active biopolymers in green non-conventional media: a sustainable tool for developing clean chemical processes
- Author
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Juana M. Bernal, Celia Gomez, Eduardo García-Verdugo, Pedro Lozano, Santiago V. Luis, and Susana Nieto
- Subjects
Chemical process ,biocatalyst ,RNA Stability ,Ionic Liquids ,Reuse ,Chemical reaction ,chemistry.chemical_compound ,Biopolymers ,biopolymer ,catalytic efficiency ,Materials Chemistry ,Organic chemistry ,RNA, Small Interfering ,immobilized enzyme ,Supercritical carbon dioxide ,Metals and Alloys ,liquid liquid extraction ,cellulose ,Enzymes ,Surfaces, Coatings and Films ,Electronic, Optical and Magnetic Materials ,enzyme activity ,enzyme inactivation ,biotransformation ,hydrogenation ,room temperature ,chemical reaction ,biocatalysis ,Nanotechnology ,biodiesel ,engineering.material ,Catalysis ,protein conformation ,acetophenone ,packed bed reactor ,ionic liquid ,enzyme immobilization ,structure activity relation ,hydrogen bond ,supercritical fluid ,DNA degradation ,carbon dioxide ,Green Chemistry Technology ,continuous flow reactor ,DNA ,General Chemistry ,Carbon Dioxide ,palladium ,Supercritical fluid ,saccharification ,enzyme ,chemistry ,Biofuels ,Ionic liquid ,Biocatalysis ,Solvents ,Ceramics and Composites ,engineering ,Biopolymer - Abstract
The greenness of chemical processes turns around two main axes: the selectivity of catalytic transformations, and the separation of pure products. The transfer of the exquisite catalytic efficiency shown by enzymes in nature to chemical processes is an important challenge. By using appropriate reaction systems, the combination of biopolymers with supercritical carbon dioxide (scCO2) and ionic liquids (ILs) resulted in synergetic and outstanding platforms for developing (multi)catalytic green chemical processes, even under flow conditions. The stabilization of biocatalysts, together with the design of straightforward approaches for separation of pure products including the full recovery and reuse of enzymes/ILs systems, are essential elements for developing clean chemical processes. By understanding structure–function relationships of biopolymers in ILs, as well as for ILs themselves (e.g. sponge-like ionic liquids, SLILs; supported ionic liquids-like phases, SILLPs, etc.), several integral green chemical processes of (bio)catalytic transformation and pure product separation are pointed out (e.g. the biocatalytic production of biodiesel in SLILs, etc.). Other developments based on DNA/ILs systems, as pathfinder studies for further technological applications in the near future, are also considered. This work was partially supported by the Fundación SENECA-CARM 19278/PI/14, PROMETEO/2012/020 and UJI P1-1B2013-37 grants.
- Published
- 2015
44. A novel safety assessment strategy applied to non-selective extracts
- Subjects
Squash ,Food Safety ,Unclassified drug ,Food Handling ,Analytical parameters ,Carbamic acid derivative ,Nitroso derivative ,Procedures ,RAPID - Risk Analysis for Products in Development ARPC - Analytical Research (Pharm & Chemistry) ,Organophosphate ,Non selective extract ,Aflatoxin ,Methods ,Complex mixture safety assessment strategy ,Soft drink ,Chemical analysis ,Fruit juice ,Polymer ,Risk assessment ,Life Triskelion BV ,Dietary fiber ,Chemistry ,Sambucus ,Yoghurt ,allergenicity ,Threshold of toxicological concern ,Liquid liquid extraction ,Azoxy derivative ,Food composition ,Safety ,Hazard Analysis and Critical Control Points ,Healthy Living ,TTC ,Chemical compound ,Ice cream ,Strategy ,Liquid chromatography ,Mass fragmentography ,Ash ,Food Contamination ,Processing ,Complex Mixtures ,Gas Chromatography-Mass Spectrometry ,Complex mixture safety assessment ,Exposure ,Biphenyl derivative ,Humans ,Animalia ,Food and Nutrition ,Food color ,Life and Social Sciences ,Sugar ,Solid phase extraction ,Steroid ,Semi volatile substance ,Fuit gum ,Nutrition ,Toxicity ,Protein ,Volatile agent ,Drug mixture ,Water ,Non-selective extract ,Solid phase microextraction ,ELSS - Earth ,Nonhuman ,Dibenzodioxin derivative ,Prevention and control ,Food ,Concentration (parameters) ,Dibenzofuran derivative ,Miscellaneous drugs and agents ,Toxicity testing ,Comparative study ,Genotoxicity ,Hazard assessment ,Controlled study ,Analysis ,Food Analysis - Abstract
A main challenge in food safety research is to demonstrate that processing of foodstuffs does not lead to the formation of substances for which the safety upon consumption might be questioned. This is especially so since food is a complex matrix in which the analytical detection of substances, and consequent risk assessment thereof, is difficult to determine. Here, a pragmatic novel safety assessment strategy is applied to the production of non-selective extracts (NSEs), used for different purposes in food such as for colouring purposes, which are complex food mixtures prepared from reference juices. The Complex Mixture Safety Assessment Strategy (CoMSAS) is an exposure driven approach enabling to efficiently assess the safety of the NSE by focussing on newly formed substances or substances that may increase in exposure during the processing of the NSE. CoMSAS enables to distinguish toxicologically relevant from toxicologically less relevant substances, when related to their respective levels of exposure. This will reduce the amount of work needed for identification, characterisation and safety assessment of unknown substances detected at low concentration, without the need for toxicity testing using animal studies. In this paper, the CoMSAS approach has been applied for elderberry and pumpkin NSEs used for food colouring purposes.
- Published
- 2015
45. A novel safety assessment strategy applied to non-selective extracts
- Author
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Lene Munch Nielsen, Stefan Ronsmans, Sander Koster, Lisette Krul, Elwin Verheij, W.R. Leeman, Ellen Dutman, Leo van Stee, and Hub Noteborn
- Subjects
Squash ,Food Safety ,Chemical compound ,Unclassified drug ,Food Handling ,Analytical parameters ,Carbamic acid derivative ,Nitroso derivative ,Hazard analysis ,Toxicology ,Procedures ,RAPID - Risk Analysis for Products in Development ARPC - Analytical Research (Pharm & Chemistry) ,chemistry.chemical_compound ,Organophosphate ,Non selective extract ,Aflatoxin ,Methods ,Complex mixture safety assessment strategy ,Soft drink ,Chemical analysis ,Fruit juice ,Polymer ,Volume concentration ,Risk assessment ,Food colouring ,Chemistry ,General Medicine ,Life Triskelion BV ,Dietary fiber ,Food Analysis ,Sambucus ,Yoghurt ,allergenicity ,Threshold of toxicological concern ,Liquid liquid extraction ,Hazard analysis and critical control points ,Azoxy derivative ,Food composition ,Safety ,Hazard Analysis and Critical Control Points ,Healthy Living ,TTC ,Ice cream ,Strategy ,Liquid chromatography ,Mass fragmentography ,Ash ,Food Contamination ,Processing ,Complex Mixtures ,Gas Chromatography-Mass Spectrometry ,Complex mixture safety assessment ,Exposure ,Biphenyl derivative ,Humans ,Animalia ,Food and Nutrition ,Food color ,Sugar ,Solid phase extraction ,Steroid ,Semi volatile substance ,Fuit gum ,Nutrition ,Toxicity ,business.industry ,Protein ,Volatile agent ,Drug mixture ,Water ,Non-selective extract ,Solid phase microextraction ,Food safety ,Nonhuman ,Dibenzodioxin derivative ,Prevention and control ,Food ,Concentration (parameters) ,Dibenzofuran derivative ,Miscellaneous drugs and agents ,Toxicity testing ,Biochemical engineering ,Comparative study ,ELSS - Earth, Life and Social Sciences ,Genotoxicity ,business ,Hazard assessment ,Controlled study ,Analysis ,Food Science - Abstract
A main challenge in food safety research is to demonstrate that processing of foodstuffs does not lead to the formation of substances for which the safety upon consumption might be questioned. This is especially so since food is a complex matrix in which the analytical detection of substances, and consequent risk assessment thereof, is difficult to determine. Here, a pragmatic novel safety assessment strategy is applied to the production of non-selective extracts (NSEs), used for different purposes in food such as for colouring purposes, which are complex food mixtures prepared from reference juices. The Complex Mixture Safety Assessment Strategy (CoMSAS) is an exposure driven approach enabling to efficiently assess the safety of the NSE by focussing on newly formed substances or substances that may increase in exposure during the processing of the NSE. CoMSAS enables to distinguish toxicologically relevant from toxicologically less relevant substances, when related to their respective levels of exposure. This will reduce the amount of work needed for identification, characterisation and safety assessment of unknown substances detected at low concentration, without the need for toxicity testing using animal studies. In this paper, the CoMSAS approach has been applied for elderberry and pumpkin NSEs used for food colouring purposes.
- Published
- 2015
46. Analytical possibilities for the detection of stanozolol and its metabolites
- Author
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C. Van Poucke, L.A. van Ginkel, M Dubois, G. Pottie, Mirjam Nielen, K De Wasch, S. Poelmans, R. Schilt, Saskia S. Sterk, Sandra Impens, M Van de Wiele, T Hamoir, C. Van Peteghem, Ph. Delahaut, Dirk Courtheyn, J Vercammen, Rainer W. Stephany, and H.F. De Brabander
- Subjects
medicine.medical_treatment ,Metabolite ,gas chromatography ,Urine ,Biochemistry ,Analytical Chemistry ,chemistry.chemical_compound ,Liquid chromatography–mass spectrometry ,Metabolites ,Solid phase extraction ,anabolic steroids ,Spectroscopy ,Stanozolol ,conference paper ,metabolites ,mass spectrometry ,Chemistry ,liquid liquid extraction ,RIKILT - Analytical Services & Development ,urine ,hydrolysis ,priority journal ,Health ,GC-MS ,immunoaffinity chromatography ,medicine.drug ,kidney clearance ,metabolite ,urinary excretion ,chemistry ,medicine ,Environmental Chemistry ,liquid chromatography ,Animalia ,chemical compound ,Analytical research ,Chromatography ,nonhuman ,literature ,solid phase extraction ,stanozolol ,drug metabolism ,LC-MS ,Anabolic steroids ,anabolic agent ,drug blood level ,extraction ,Gas chromatography ,Gas chromatography–mass spectrometry ,Anabolic steroid - Abstract
In sports doping, as well in man as in horseracing, stanozolol (Stan) was abused and became the subject of metabolism research. Also in veterinary practice, stanozolol became an important misused anabolic steroid. Like most other anabolic steroids, stanozolol has poor gas chromatographic behavior. It is difficult to detect in urine, because of low urinary excretion and renal clearance. This is due to the rapid metabolization, leading to low concentration levels of the parent compound found in urine. Therefore, most research studies have focused on the detection of its urinary metabolites. For the identification of the metabolites, different methods of extraction and detection are described in the literature. These are reviewed in this article. Most authors use a hydrolysis to free the phase II metabolites. Extraction procedures vary from solid-phase extraction (SPE), liquid-liquid (L-L) extraction to immunoaffinity chromatography (IAC). For the final detection, the use of gas chromatography (GC)-mass spectrometry (MS) can be compared with liquid chromatography (LC)-MSn. Different metabolites are identified depending on the administration of stanozolol in the animal experiment (oral or intramuscular). Analyses for these analytes in other matrices are also briefly discussed. © 2002 Elsevier Science B.V. All rights reserved.
- Published
- 2002
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47. Rapid confirmatory analysis of avermectin residues in milk by liquid chromatography tandem mass spectrometry
- Author
-
Tahir Kahraman and Nurullah Ozdemir
- Subjects
Electrospray ionization ,limit of quantitation ,lcsh:TX341-641 ,Tandem mass spectrometry ,01 natural sciences ,Article ,evaporation ,chemistry.chemical_compound ,Liquid chromatography–mass spectrometry ,residue ,tandem mass spectrometry ,medicine ,liquid chromatography ,quantitative study ,Doramectin ,Avermectin ,Detection limit ,Pharmacology ,milk ,Chromatography ,limit of detection ,nonhuman ,010405 organic chemistry ,bovine ,010401 analytical chemistry ,lcsh:RM1-950 ,liquid liquid extraction ,doramectin ,avermectin ,0104 chemical sciences ,Moxidectin ,unclassified drug ,acetonitrile ,ivermectin b1a ,lcsh:Therapeutics. Pharmacology ,chemistry ,abamectin b1a ,eprinomectin b1a ,validation study ,Abamectin ,moxidectin ,avermectin derivative ,electrospray ,liquid chromatography/tandem mass spectrometry ,lcsh:Nutrition. Foods and food supply ,medicine.drug ,Food Science - Abstract
Our study developed a quick method for confirmatory analysis of avermectins (abamectin B1a, doramectin, ivermectin B1a, eprinomectin B1a, and moxidectin) in bovine milk according to the European Commission Decision 2002/657/EC requirements. Avermectins were liquid-liquid extracted with acetonitrile, followed by an evaporation step, and then analyzed by liquid chromatography/electrospray ionization tandem mass spectrometry in the negative ion mode. An in-house method validation was performed and the data reported on specificity, linearity, recovery, limit of detection, limit of quantitation, decision limit, and detection capability. The advantage of this method is that low levels of avermectins are detectable and quantitatively confirmed at a rapid rate in milk. © 2015, Food and Drug Administration, Taiwan. Published by Elsevier Taiwan LLC.
- Published
- 2014
48. Estimation of pesticide residues in fruits, vegetables and water
- Author
-
Pragti Kumari, H. N. Sharma, Yogesh Singh, L. P. Srivastava, Nisha Srivastava, Sonam kumari, and Pawan Kumar
- Subjects
Gas chromatography ,lcsh:Biology (General) ,Liquid liquid extraction ,lcsh:QR1-502 ,Pesticides ,lcsh:QH301-705.5 ,lcsh:Microbiology ,QuEChERS method - Abstract
Nowadays, pesticide use is on increase day by day in every field of life like agriculture, household and in industry. Most of the pesticides are not biodegradable and those which are degradable cannot degrade completely. Hence, they reach to our fruits, vegetables, grains and water bodies. Even after washing the pesticide residues left in our foodstuffs. Since last decade, it has been observed that analysed pesticide residues were either BDL or < MRL in the majority of samples. In this study vegetable, fruits and grains are an important food item and proper care should be taken to use the very safe pesticide fort avoiding potential risks to human. It is, therefore, suggested that the food item collected from in and around Lucknow City, India is comparatively safe from pesticide residues. A periodical monitoring of pesticide residues in other food commodities is the recent need for the consumers as well as authorities of food quality control.
- Published
- 2014
49. Spectrophotometric determination of nitrogen dioxide, nitrite and nitrate with Neutral Red
- Author
-
N. Balasubramanian and N. Gayathri
- Subjects
Neutral red ,nitrogen dioxide ,Inorganic chemistry ,General Engineering ,liquid liquid extraction ,General Chemistry ,Molar absorptivity ,chemistry.chemical_compound ,chemistry ,Nitrate ,nitrate ,Bromide ,chemical analysis ,Triethanolamine ,medicine ,spectrophotometry ,Nitrogen dioxide ,Nitrite ,Absorption (chemistry) ,nitrite ,neutral red ,absorption ,deamination ,medicine.drug - Abstract
A simple and sensitive spectrophotometric method for the determination of nitrogen dioxide in air and nitrite in water, soil, some analytical grade chemicals and tooth paste has been developed. Nitrogen dioxide in air is fixed as nitrite ion in alk a- line sodium arsenite or triethanolamine absorber solution. The method is based on the reaction of nitrite in aqueous medium wit h known excess of Neutral Red (C.I. 50040), an azine dye having a primary amino group with absorption maxima at 530 nm. In acid medium, it showed a decrease in colour intensity due to diazotization, followed by deamination. Addition of bromide ion enhances the rate of diazotization, and the reaction goes to completion almost instantaneously. Beer's law is obeyed over the range 0 - 20 µg nitrite and the molar absorptivity is 2.5 〈 104 L mol-1 cm-1. The colour system is stable for 2 days. The dye can be extracted under alkaline condition in iso-amyl alcohol and the addition of methanolic sulphuric acid restores the dye co lour. It showed molar absorptivity of 4.3 〈 104 L mol-1 cm-1. Beer's law is obeyed over the range 0 - 1.6 µg of nitrite, having a detec- tion limit of 0.15 µg.
- Published
- 1999
- Full Text
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50. A novel safety assessment strategy applied to non-selective extracts
- Author
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Koster, S., Leeman, W.R., Verheij, E.R., Dutman, A.E., Stee, L.L.P. van, Munch Nielsen, L., Ronsmans, S., Noteborn, H., Krul, L., Koster, S., Leeman, W.R., Verheij, E.R., Dutman, A.E., Stee, L.L.P. van, Munch Nielsen, L., Ronsmans, S., Noteborn, H., and Krul, L.
- Abstract
A main challenge in food safety research is to demonstrate that processing of foodstuffs does not lead to the formation of substances for which the safety upon consumption might be questioned. This is especially so since food is a complex matrix in which the analytical detection of substances, and consequent risk assessment thereof, is difficult to determine. Here, a pragmatic novel safety assessment strategy is applied to the production of non-selective extracts (NSEs), used for different purposes in food such as for colouring purposes, which are complex food mixtures prepared from reference juices. The Complex Mixture Safety Assessment Strategy (CoMSAS) is an exposure driven approach enabling to efficiently assess the safety of the NSE by focussing on newly formed substances or substances that may increase in exposure during the processing of the NSE. CoMSAS enables to distinguish toxicologically relevant from toxicologically less relevant substances, when related to their respective levels of exposure. This will reduce the amount of work needed for identification, characterisation and safety assessment of unknown substances detected at low concentration, without the need for toxicity testing using animal studies. In this paper, the CoMSAS approach has been applied for elderberry and pumpkin NSEs used for food colouring purposes.
- Published
- 2015
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