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Metal ion pollution poses a global concern due to its significant risks to both human health and environmental well-being. The toxicity of these ions can increase when they coexist, interacting with each other and with other harmful substances, even at low concentrations. Therefore, an accurate, rapid, and cost-effective methodology is urgently needed for the simultaneous quantification of multiple metal ions. This study presents a new approach for the multiplexed detection of various metal ions (Ag + , Cu 2+ , Hg 2+ , Al 3+ , Pb 2+ , Fe 3+ , Fe 2+ , Zn 2+ , Ni 2+ , Cd 2+ , and Ca 2+ ) using a triple-emission nanoprobe comprising carbon dots and distinctly capped CdTe quantum dots, specifically green-emitting glutathione -quantum dots and red-emitting 3-mercaptopropionic acid-quantum dots. The method achieved high accuracy by analysing first- and second-order photoluminescence data with distinct advanced chemometric tools. R 2 P values for partial least squares and unfolded partial least square models exceeding 0.9 for several metal ions at low concentrations (mmol L -1 ) were obtained. Additionally, PL second-order data yielded significantly better results than PL first-order data, attributed to the distinct behaviour of the metal ions over time. Interestingly, it was also noted for the first time the significant contribution of the molar ratio between the metal ions on the models' accuracy. This novel method provides a highly accurate and efficient way to detect multiple metal ions simultaneously, paving the way for improved environmental monitoring and pollution assessment. The utilization of the proposed method contributes to a better understanding of the complex interactions in mixed metal ion systems, allowing for earlier detection and mitigation of metal ion contamination threats., Competing Interests: Declarations. Conflict of interest: The authors declare no competing interests., (© 2024. The Author(s).)

Chronic wounds (CW) present a significant healthcare challenge due to their prolonged healing time and associated complications. To effectively treat these wounds and prevent further deterioration, monitoring their healing progress is crucial. Traditional wound assessment methods relying on visual inspection and subjective evaluation are prone to inter-observer variability. Biomarkers play a critical role in objectively evaluating wound status and predicting healing outcomes, providing quantitative measures of wound healing progress, inflammation, infection, and tissue regeneration. Recent attention has been devoted to identifying and validating CW biomarkers. Various studies have investigated potential biomarkers, including growth factors, cytokines, proteases, and extracellular matrix components, shedding light on the complex molecular and cellular processes within CW. This knowledge enables a more targeted and personalized approach to wound management. Accurate and sensitive techniques are necessary for detecting CW biomarkers. Thus, this review compares and discusses the use of electrochemical and optical sensors for biomarker determination. The advantages and disadvantages of these sensors are highlighted. Differences in detection capabilities and characteristics such as non-invasiveness, portability, high sensitivity, specificity, simplicity, cost-effectiveness, compatibility with point-of-care applications, and real-time monitoring of wound biomarkers will be pointed out and compared. In summary, this work provides an overview of CW, explores the emerging field of CW biomarkers, and discusses methods for detecting these biomarkers, with a specific focus on optical and electrochemical sensors. The potential of further research and development in this field for advancing wound care and improving patient outcomes will also be noted., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier B.V. All rights reserved.)

The combination of multiple quantum dots (QDs) in a multi-emitter nanoprobe can be envisaged as a promising sensing scheme, as it enables obtaining a collective response of individual emitters towards a given analyte and allows for achieving specific analyte-response profiles. The processing of these profiles using adequate chemometric methods empowers a more sensitive, reliable and selective determination of the target analyte. In this work, we developed a kinetic fluorometric method consisting of a dual CdTe/AgInS 2 quantum dots photoluminescence probe for the determination of acetylsalicylic acid (ASA). The fluorometric response was acquired as second-order time-based excitation/emission matrices that were subsequently processed using chemometric methods seeking to assure the second-order advantage. The data obtained in this work are considered second-order data as they have a three-dimensional size, I × J × K (where I represents the samples' number, J the fluorescence emission wavelength while K represents the time). In order to select the most adequate chemometric method regarding the obtained data structure, different chemometric models were tested, namely unfolded partial least squares (U-PLS), N-way partial least squares (N-PLS), multilayer feed-forward neural networks (MLF-NNs) and radial basis function neural networks (RBF-NNs).

Saccharomyces cerevisiae has been used as a eukaryotic model organism for studying the toxic effects of various compounds. In this context, an automated spectrophotometric method based on the enzymatic reduction of methylene blue dye to a colorless product by living yeast cells was implemented in a sequential injection analysis system. Loss of yeast viability/impaired metabolic activity was monitored by an increase in optical density at 664 nm. To prove the usefulness of this approach, the toxicity of ILs (ionic liquids), GUMBOS (group of uniform materials based on organic salts), and DESs (deep eutectic solvents) was examined. Differences obtained between IC 50 values confirmed the impact of structural elements on each compounds' toxicity. While DESs appeared to be less toxic than ILs, GUMBOS were found to be among the most toxic compounds to yeast cells and thus can be viewed as promising antimicrobial candidates. The automated methodology showed satisfactory repeatability and reproducibility (RSD < 9%), which is in good agreement with Green Chemistry principles. In fact, the method required consumption of only 40 μL of reagents and produced less than 2 mL of effluents per cycle. Thus, the developed assay can be used as an alternative tool for toxicity screening., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Background: The epidural ligaments (ELs) (of Hofmann) were described as fibrous bands interconnecting the ventrolateral spinal dura and the posterior longitudinal ligament below L1. They are hardly ever discussed in the literature or considered in hypothesis-driven basic science experiments or spine biomechanical models., Methods: Intraoperative photographs were obtained to illustrate a group of posterolateral spinal ELs. In addition, electronic database searches (PubMed, Ovid Embase, and SCOPUS) were utilized to summarize the anatomy, and relevant clinical and surgical factors impacting these ELs., Results: ELs attach circumferentially at most spinal levels. They anchor the nerve root sleeves ventrally, and therefore, may play a role in the some idiopathic neurologic deficits (e.g., postoperative radiculopathies, C5 palsies) in patients without radiological compression. The posterolateral ELs originate on the dura dorsal to the nerve root sleeves and insert on the ipsilateral lamina, interlaminar ligament, and facet capsule. They appear to be continuous with the peridural membrane, a fibrovascular sheath that surrounds the thecal sac and serves as a scaffold for the internal vertebral venous plexus of Batson and epidural fat., Conclusion: The spinal ELs should be divided sharply during surgery to prevent durotomies, especially in patients with advanced spondylosis and facet arthropathy. Disconnecting these ligaments releases the thecal sac laterally and ventrally, allowing for medial mobilization when performing discectomies or for working in the ventral epidural space., Competing Interests: There are no conflicts of interest., (Copyright: © 2020 Surgical Neurology International.)

A highly sensitive fluorescence detection probe was developed by tailoring plastic antibodies on the external surface of aqueous soluble quantum dots (QDs). The target was Myoglobin (Myo), a cardiac biomarker that quenched the intrinsic fluorescent emission of cadmium telluride (CdTe) QDs capped with mercaptopropionic acid (CdTe-MPA-QDs). The QDs were incubated with the target protein and further modified with a molecularly-imprinted polymer (MIP) produced by radical polymerization of acrylamide and bisacrylamide. The main physical features of the materials were assessed by electron microscopy, dynamic light scattering (DLS), UV/Vis spectrophotometry and spectrofluorimetry. The plastic antibodies enabled Myo rebinding into the QDs with subsequent fluorescence quenching. This QD-probe could detect Myo concentrations from 0.304 to 571 pg/ml (50.6 fM to 95 pM), with a limit of detection of 0.045 pg/ml (7.6 fM). The proposed method was applied to the determination of Myo concentrations in synthetic human serum. The results obtained demonstrated the ability of the modified-QDs to determine Myo below the cut-off values of myocardial infarction. Overall, the nanostructured MIP-QDs reported herein displayed quick responses, good stability and sensitivity, and high selectivity for Myo, offering the potential to be explored as new emerging sensors for protein detection in human samples.

A multivariate spectrophotometric method is a potential approach that enables discrimination of spectra of components in complex matrices (e.g., pharmaceutical formulation) serving as a substitution method for chromatography. Four green smart multivariate spectrophotometric models were proposed and validated, including principal component regression (PCR), partial least-squares (PLS), multivariate curve resolution-alternating least squares (MCR-ALS), and artificial neural networks (ANN). The developed chemometric models were compared to resolve highly overlapping spectra of Paracetamol (PARA), Chlorpheniramine maleate (CPM), Caffeine (CAF), and Ascorbic acid (ASC). The four multivariate calibration models were assessed via recoveries percent, and root mean square error of prediction. Hence, the proposed models were efficiently applied with no need for any preliminary separation step. The models were utilized to analyze the studied components in their combined pharmaceutical formulation (Grippostad® C capsules). Analytical GREEnness Metric Approach (AGREE) and eco-scale tools were applied to assess the greenness of the established models and found to be 0.77 and 85, respectively. Moreover, the proposed models have been compared to official ones showing no considerable variations in accuracy and precision. Therefore, these models can be highly advantageous for conducting standard pharmaceutical analysis of the substances researched within product testing laboratories. [ABSTRACT FROM AUTHOR]

Heavy metal ions bioaccumulation can cause severe damage to environment and human health. Hence, the development of an effective detection assay of trace amounts of these ions is of great importance. Here, CdTe quantum dots (QDs) capped with mercaptosuccinic acid (MSA) ligands have been synthesized in aqueous solution with significant stability and good fluorescence properties. Photophysical characterization was performed using FTIR, XRD, HRTEM and UV–Vis. Absorption, PL and PLRT techniques, seeking their subsequent application as fluorescent probes for metal cations. CdTe-MSA QDs showed selective sensitivity toward Hg2+ ions by monitoring quantitative fluorescence quenching with increasing analyte content. Under optimal conditions, the linear range for the detection was 0.2–6 μM with a detection limit of 0.05 μM. According to the Stern–Volmer model, it can be inferred that a static quenching mechanism via Hg2+ selective binding to MSA carboxylate groups is operating with electron transfer process. Excess of mercuric ions further decreased and red shifted the fluorescence possibly due to competitive cation exchanges. To further explain the corresponding ligation mechanisms, adsorption behavior study was conducted via several isotherms as well as statistical physics models. The pseudo-first-order model can describe the adsorption kinetics of Hg2+ on CdTe-MSA QDs more accurately and the experimental data fitted well the Langmuir isotherm model of monolayer adsorption on homogeneous surface. Furthermore, this spontaneous process conforms to the Hill model as a physisorption with an adsorption energy of 32 kJ.mol−1 associated with the electrostatic interactions and hydrogen bonding. The developed system was assayed in the Hg2+ trace amount detection in real tap water and showed satisfactory accuracy performance meeting analytical requirements. The relevant results demonstrated that CdTe-MSA QDs could be deployed as promising Hg2+ fluorescent chemosensing system with high sensitivity and selectivity over wide linear detection range that have great potential for real water samples analysis. [ABSTRACT FROM AUTHOR]

Single quantum dots (Qdots) are often used in the field of single-molecule imaging. Qdots are sensitive to changes in the physical interactions between the Qdots and the surrounding materials. However, the spectral changes in a single Qdot emission have not been studied in detail. Low-temperature plasma treatment of glass surfaces reduced the intensity of the 655 nm emission peak of Qdot655 on glass surfaces, but did not significantly change the intensity of the 580 nm emission. Silanization of the glass surface increases the thickness of the silane layer, and the 655 nm emission peak increased. When single Qdots on the untreated glass were imaged, plasma treatment decreased the intensity of red emission and increased yellow emission. When Qdots were brought close to the glass surface in the range of 28–0 nm, the red emission intensity decreased and the yellow emission intensity increased slightly. When single actin filaments were labeled with Qdots, fluctuations of the yellow and red emission of the Qdot were detected, which reflected the very small distance changes. Our results indicate that the local interaction of Qdots with the glass surface improves the spatial and temporal resolution of optical measurements of biomolecules labeled with Qdots. [ABSTRACT FROM AUTHOR]

Luminescent semiconductor quantum dots (QDs) are frequently used in the life and material sciences as reporter for bioimaging studies and as active components in devices such as displays, light-emitting diodes, solar cells, and sensors. Increasing concerns regarding the use of toxic elements like cadmium and lead, and hazardous organic solvents during QD synthesis have meanwhile triggered the search for heavy-metal free QDs using green chemistry syntheses methods. Interesting candidates are ternary AgInS2 (AIS) QDs that exhibit broad photoluminescence (PL) bands, large effective Stokes shifts, high PL quantum yields (PL QYs), and long PL lifetimes, which are particularly beneficial for applications such as bioimaging, white light-emitting diodes, and solar concentrators. In addition, these nanomaterials can be prepared in high quality with a microwave-assisted (MW) synthesis in aqueous solution. The homogeneous heat diffusion and instant temperature rise of the MW synthesis enables a better control of QD nucleation and growth and thus increases the batch-to-batch reproducibility. In this study, we systematically explored the MW synthesis of AIS/ZnS QDs by varying parameters such as the order of reagent addition, precursor concentration, and type of stabilizing thiol ligand, and assessed their influence on the optical properties of the resulting AIS/ZnS QDs. Under optimized synthesis conditions, water-soluble AIS/ZnS QDs with a PL QY of 65% and excellent colloidal and long-term stability could be reproducible prepared. [ABSTRACT FROM AUTHOR]

Pesticides that linger in the environment and ecosystems for an extended period can cause severe and dangerous health problems in humans. To detect pesticides in foods, the development of high-sensitivity and quick screening technologies was required. This research investigated the performance of Au@Ag NPs with varying thicknesses of the silver shell for detecting trace quantities of thiabendazole (TBZ) in apples using surface-enhanced Raman spectroscopy (SERS). The Au@Ag NPs were synthesized by coating 32 nm gold seeds with different thicknesses of silver shell ranging from 2.4 to 8.7 nm, achieved by adjusting the incorporation of AgNO 3 and ascorbic acid. The optimized Au@Ag NPs with a 7.3 nm silver shell demonstrated outstanding SERS activity, high sensitivity, and a detection limit of 0.05 μg/mL for TBZ. The R 2 values, representing the goodness of fit, were found to be 0.990 and 0.986 for standard and real TBZ samples, respectively, indicating a strong correlation between the measured signal and the TBZ concentration. The recovery analysis showed a reliable and accurate detection capability (96 to 105%), suggesting good reliability and accuracy of the SERS-based detection using the optimal Au@Ag NPs. Overall, this research highlights the potential of SERS with optimal Au@Ag NPs for rapid and effective monitoring of pesticides in the food industry., (© 2023. The Author(s), under exclusive licence to Springer-Verlag GmbH, DE part of Springer Nature.)

Background: With the rapid development of nanotechnology, more and more nanoproducts are being released into the environment where they may both pose ecological risks and be toxic to living organisms. The ecotoxicological impact of quantum dots (QDs), a class of nanoparticles (NPs), on aquatic organisms is becoming an emerging issue, this due to their nano-specific properties, to the physico-chemical transformation in the environment and to the possible release of toxic metals from their structure such as Cd. Methods: In this work, (i) spectroscopic measurements of commercially available Cd-based QDs (CdSe/ZnS-COOH) were made at various pH values (5.0 and 7.0) to study their interactions (at a concentration of 4 nm) with various strains of Gram-positive and Gram-negative gut bacteria after short-term exposure and (ii) the antibacterial efficacy of QDs and Cd2+ (at a concentration 0.09-3.56 mM) against gut bacteria isolated from wild freshwater Salmo trutta fry was studied at different temperatures (15 °C and 25 °C) and pH values (5.0 and 7.0) by applying a well-established disc diffusion assay. Results: Twenty-six gut bacterial isolates from wild Salmo trutta fry were identified as Aeromonas spp., A. popoffii, A. salmonicida, A. sobria, Carnobacterium maltaromaticum, Buttiauxella sp., Listeria sp., Microbacterium sp., Shewanella putrefaciens and Serratia sp. Cd-based (CdSe/ZnS-COOH) QDs at a concentration of 4 nm were found to be stable in aqueous media (with pH 7.0) or starting to form aggregates (at pH 5.0), thus, apparently, did not release heavy metals (HMs) into the media over 48 h in conditions of light or dark and did not show antibacterial efficacy on the gut bacteria isolated from wild Salmo trutta fry after short-term (9 h and 48 h) incubations. Cd2+ was found to produce significant dose-dependent toxic effects on bacterial growth, and the size of the inhibition zones on some of the tested strains significantly correlated with temperature. The most sensitive and the most resistant to Cd2+ were the Gram-positive bacteria, for which the minimum inhibitory concentration (MIC) values of Cd2+ were 0.09-0.27 mM and 3.11-3.29 mM respectively and varied significantly between the tested temperatures (15 °C and 25 °C). The MIC values of Cd2+ for the Gram-negative bacteria (18 out of 22 strains) ranged from 0.44 to 0.71 mM and did not differ significantly between the tested temperatures. Among the selected Gram-positive and Gram-negative strains, those with the higher sensitivity towards Cd2+ also revealed relatively stronger signals of QDs photoluminescence (PL) when transferred after incubation into fresh medium without QDs. In addition, the formation of endogenous metalloporphyrins observed spectroscopically in some bacterial strains indicates certain differences in metabolic activity that may play a protective role against potential oxidative damage. [ABSTRACT FROM AUTHOR]

A new bioanalytical labeling system based on alloyed quantum dots' (QDs) photoluminescence quenching caused by an enzymatic reaction has been developed and tested for the first time. The catalytic role of the enzyme provides high sensitivity and the possibility of varying detecting time to improve assay sensitivity. Alloyed luminescent QDs were chosen in view of their small size (5–7 nm) and the high sensitivity of their optical properties to physicochemical interactions. Here, we described the synthesis of alloyed luminescent QDs and demonstrated the possibility of using them as a luminescent turn-off substrate for enzymatic assay. Synthesized alloyed QDs were found to be a sensitive turn-off substrate for glucose oxidase in homogeneous and heterogeneous assay models. CdZnSeS and CdZnSeS/ZnS QDs covered with dihydrolipoic acid and 2-mercaptoethanol were tested. A glucose oxidase limit of detection of 6.6 nM for the heterogenous high-throughput model assay was reached. [ABSTRACT FROM AUTHOR]

A novel procedure has been developed for spectrophotometric determination of anionic surfactants in water using a solenoid micro-pump as fluid-propulsion device. The proposed method is based on substitution of methyl orange (MO) by anionic surfactants in the formation of an ion-pair with the cetyl pyridine ion (CPC+) at pH 5.0. The flow network comprised four solenoid micro-pumps which, under microcomputer control, enabled sample and reagent introduction, and homogenisation in the reaction zone. The system is flexible and simple to operate and control, and sensitive and precise. The analytical plot for the anionic surfactant was linear between 1.43×10-6 and 1.43×10-5 mol L-1 (0.5 to 5.0 mg L-1;R=0.997,n=5). The relative standard deviation was 0.8% (n=11) for a sample containing 5.74×10-6 mol L-1 (2 mg L-1) surfactant. The limit of detection was 9.76×10-8 mol L-1 (0.034 mg L-1) and the sampling throughput was 60 determinations per hour. The results obtained for washing-water samples were comparable with those obtained by use of the reference method, and no significant differences at the 95% confidence level were observed. [ABSTRACT FROM AUTHOR]

Biophoton radiation also referred to as ultra-weak photon emission (UPE) is used to denote a spontaneous and permanent photon emission associated with oxidative processes in cells and seems to universally occur in all living systems as a result of the generation of reactive oxygen species (ROS) that are produced under stress conditions. The measurement of this biophoton emission allows for a non-invasive approach in monitoring phenological stages throughout plant development which has direct relevance in agriculture research. In this study, the emission of photons emanating from sunflower (Helianthus annuus, L.) plants exposed to biotic and abiotic stress has been investigated. In healthy plants raised under controlled growth conditions UPE was low whereas in stressed individuals it considerably increased; particularly upon water stress. The kinetics of the signal is shown to reveal an exponential decay with characteristic dynamics, which appears to reflect different physiological states concomitantly setting in upon stress. The dynamics of the signal decay is shown to vary according to the type of stress applied (biotic vs. abiotic) hence suggesting a putative relationship between the kinetic traits of change in the signal intensity-decay and stress. Intriguingly, the determination of the change in the intensity of biophoton emission that ensued in a short time course was possible by using the initial biophoton emission intensity. The predictability level of the equations demonstrated the applicability of the model in a corroborative manner when employing it in independent UPE-measurements, thus permitting to forecast the intensity change in a very accurate way over a short time course. Our findings allow the notion that albeit stress confers complex and complicated changes on oxidative metabolism in biological systems, the employment of biophoton imaging offers a feasible method making it possible to monitor oxidative processes triggered by stress in a non-invasive and label-free way which has versatile applications especially in precision agriculture. [ABSTRACT FROM AUTHOR]

Photodynamic therapy (PDT) is a well-established therapeutic for the treatment of different diseases. The growing interest of this technique required the development of new photosensitizers with better photo-features. This work reports the study of the potential of five nature-inspired amino-based flavylium compounds with different structural features as photosensitizers towards topical PDT. In terms of dark cytotoxicity the five pigments were tested towards confluent skin cells in both fibroblasts and keratinocytes. In the range of concentrations tested (6.3–100 μM), keratinocytes were more prone to growth inhibition and the IC50 values for 5OH4′NMe2, 7NEt2st4′NMe2 and 7NEt24′NH2 were determined to be 47.3 ± 0.3 μM; 91.0 ± 0.8 μM and 29.8 ± 0.8 μM, respectively. 7NEt24′NMe2, 7NEt2st4′NMe2 and 7NEt24′NH2 showed significant fluorescence quantum yields (from 3.40 to 20.20%) and production of singlet oxygen (1O2). These latter chromophores presented IC50 values of growth inhibition of keratinocytes between 0.9 and 1.5 µM, after 10 min of photoactivation with white light. This cellular damage in keratinocyte cells upon white light activation was accompanied with the production of reactive oxygen species (ROS). It was also found that the compounds can induce damage by either type I (ROS production) or type II (singlet oxygen) PDT mechanism, although a higher cell survival was observed in the presence of 1O2 quenchers. Overall, a structure–activity relationship could be established, ranking the most important functional groups for the photoactivation efficiency as follows: C7-diethylamino > C4′-dimethylamino > C2-styryl. [ABSTRACT FROM AUTHOR]

Nanozymes were the novel research field to replace natural enzymes because of stability and low cost. However, the research on nanozymes was mainly focused on peroxidase, and there was little research about nanozymes with oxidase-like activity, especially mimic oxidase of small molecules related to human physiology. High levels of uric acid (UA) in the body can cause hyperuricemia and gout. And natural uricase cured this disease because it could oxidize UA. The oxidase-like activity of mixed valence state metal organic frameworks with cerium (MVSM) had been studied, but MVSM was found to have uricase-like activity in this article. The catalytic process of UA with MVSM was studied by a variety of analytical methods, which was similar to the natural uricase except for further oxidation of H2O2. The catalytic activity constants of MVSM were acquired by the Michaelis-Menten equation. MVSM had a better ability to catalyze UA in in vivo and in vitro experiments. An enzyme-free analysis–based mimic uricase for UA was established. All the experimental results proved that MVSM had a good prospect to replace the natural uricase. [ABSTRACT FROM AUTHOR]

Increasing evidence supports the critical role of saccharides in various pathophysiological steps of tumor progression, where they regulate tumor proliferation, invasion, hematogenic metastasis, and angiogenesis. The identification and recognition of these saccharides provide a solid foundation for the development of targeted drug preparations, which are however not fully understood due to their complex and similar structures. In order to achieve fluorescence sensing of saccharides, extensive research has been conducted to design molecular probes and nanoparticles made of different materials. This paper aims to provide in-depth discussion of three main topics that cover the current status of the carbohydrate sensing based on the fluorescence sensing mechanism, including a phenylboronic acid-based sensing platform, non-boronic acid entities, as well as an enzyme-based sensing platform. It also highlights efforts made to understand the recognition mechanisms and improve the sensing properties of these systems. Finally, we present the challenge of achieving high selectivity and sensitivity recognition of saccharides, and suggest possible future avenues for exploration., (© 2023. Springer-Verlag GmbH Germany, part of Springer Nature.)

Herein, we synthesized and characterized glutathione-capped copper nanoclusters (CuNCs) using a convenient one-pot chemical reduction approach based on glutathione as capping and reducing agents. The Ce(III) induced aggregation-induced emission of CuNCs to form a CuNCs-Ce3+ fluoroprobe due to electrostatic and coordination interactions between Ce3+ and CuNCs. In contrast to CuNCs, the fluorescent intensities (FLs) of CuNCs-Ce3+ were enhanced by ~ 40-fold concomitant with 20-nm blue-shift of the maximum emission, and a 3.45-fold lengthening of the average fluorescent lifetime. The FLs of CuNCs-Ce3+ were selectively quenched at 650 nm by hydrogen peroxide (H2O2) via the redox reaction. Based on this phenomenon, the sensitive assay of H2O2 was realized, and the linear range spanned over the range of 14–140 μM. Notably, the visualization of the fluorescence quenched effect of H2O2 could be easily attained. Additionally, glucose could be specifically oxidized by glucose oxidase to produce H2O2, and thus the detection of glucose was achieved according to changes in the concentrations of H2O2. Under optimized conditions, the fluorescent assay of glucose based on the CuNCs-Ce3+ system offered the linear range of 8–48 μM with detection limit of 2.4 μM. Meanwhile, high selectivity of the as-constructed fluorescent assay allows the sensitive detection of H2O2 and glucose in real-world care products and human serum samples, showing a great application potential in their conventional monitoring. [ABSTRACT FROM AUTHOR]

The bacterial strain, EMM-1, was isolated from the rhizosphere of red maize ("Rojo Criollo") and identified as Pseudomonas protegens EMM-1 based on phylogenetic analysis of 16S rDNA, rpoB, rpoD, and gyrB gene sequences. We uncovered genes involved in the production of antimicrobial compounds like 2,4-diacetylphloroglucinol (2,4-DAPG), pyoluteorin, and lectin-like bacteriocins. These antimicrobial compounds are also produced by other fluorescent pseudomonads alike P. protegens. Double-layer agar assay showed that P. protegens EMM-1 inhibited the growth of several multidrug-resistant (MDR) bacteria, especially clinical isolates of the genera Klebsiella and β-hemolytic Streptococcus. This strain also displayed inhibitory effects against diverse fungi, such as Aspergillus, Botrytis, and Fusarium. Besides, a crude extract of inhibitory substances secreted into agar was obtained after the cold-leaching process, and physicochemical characterization was performed. The partially purified inhibitory substances produced by P. protegens EMM-1 inhibited the growth of Streptococcus sp. and Microbacterium sp., but no inhibitory effect was noted for other bacterial or fungal strains. The molecular weight determined after ultrafiltration was between 3 and 10 kDa. The inhibitory activity was thermally stable up to 60°C (but completely lost at 100°C), and the inhibitory activity remained active in a wide pH range (from 3 to 9). After treatment with a protease from Bacillus licheniformis, the inhibitory activity was decreased by 90%, suggesting the presence of proteic natural compounds. All these findings suggested that P. protegens EMM-1 is a potential source of antimicrobials to be used against pathogens for humans and plants. [ABSTRACT FROM AUTHOR]

The great interest in compounds that present antioxidant capacity has generating the urgent need for analytical methods that could determine the antioxidant potential of these sources. A method based on generation of reactive oxygen species in water from catalyst composed of palygorskita-TiO2 and silver nanoparticles (AgNPs/TiO2-PAL) was developed and applied to antioxidant assays. Silver nanoparticles were synthesized using silver nitrate solution, sodium borohydride reducing agent and Caraia gum as stabilizing agent. Incorporation of AgNPs into the previously synthesized TiO2-PAL was performed. The catalyst AgNPs/TiO2-PAL was characterized by UV–vis spectroscopy, X-ray diffractometry and scanning electron microscopy. The catalyst AgNPs/TiO2-PAL were used to perform an antioxidant activity method which consisted in monitoring the discoloration of acid yellow 73 dye (AY73) in the presence of gallic acid antioxidant comparing to the dye discoloration in the absence of the antioxidant. A microplate reader was used to measure the discoloration of the aqueous solutions of AY73, irradiated by UV light for 60 min. The effect of reactive oxygen species generated by AgNPs/TiO2-PAL based in photocatalytic kinetics of AY73 dye was investigated. The oxidation of AY73 dye by photocatalysis in the system with AgNPs/TiO2-PAL catalysts was carried out mainly by the participation of O2·−, HO· and 1O2 species, in this order of importance. The results showed that the synthesis of the AgNPs/TiO2-PAL catalyst was successfully carried out and the application of this material in the development of an innovative methodology for the determination of antioxidant activity was extremely promising. [ABSTRACT FROM AUTHOR]

Here CdTe nanocrystals were grown onto mesoporous silicas. The influence of the surface areas, volumes and pore diameters of the silica matrices on the spectroscopic properties of CdTe was evaluated. Emission properties of the CdTe were found to depend on the textural properties of silicas. Electrochemical characterization of different electrodes (unmodified carbon paste, and carbon paste modified with the mesoporous silica and with CdTe anchored onto mesoporous silica) evidenced that the presence of CdTe nanocrystals lead to a significant increase of the anodic peak referring to Cu2+ detection. The electrode with optimal characteristics responded to Cu2+ in the linear range from 5.0 × 10−8 to 2.3 × 10−6 mol L−1 and the calculated limit of detection was 6.4 × 10−8 mol L−1. The method developed here proved to be efficient for monitoring Cu2+ in sugar cane spirit (cachaça), with quantitative results comparable to those obtained from Flame Atomic Absorbtion Spectroscopy. [ABSTRACT FROM AUTHOR]

Biological systems manifest continuous weak autoluminescence, which is present even in the absence of external stimuli. Since this autoluminescence arises from internal metabolic and physiological processes, several works suggested that it could carry information in the time series of the detected photon counts. However, there is little experimental work which would show any difference of this signal from random Poisson noise and some works were prone to artifacts due to lacking or improper reference signals. Here we apply rigorous statistical methods and advanced reference signals to test the hypothesis whether time series of autoluminescence from germinating mung beans display any intrinsic correlations. Utilizing the fractional Brownian bridge that employs short samples of time series in the method kernel, we suggest that the detected autoluminescence signal from mung beans is not totally random, but it seems to involve a process with a negative memory. Our results contribute to the development of the rigorous methodology of signal analysis of photonic biosignals. [ABSTRACT FROM AUTHOR]

A high-precision exact-matching quadruple isotope dilution method (ID4MS) was employed for the quantitation of nitrate in an air-dried spinach powder Certified Reference Material (CRM). The analyte was extracted in hot water following addition of 15NO 3 − internal standard. The blend was then treated with sulfamic acid to remove nitrite and with triethyloxonium tetrafluoroborate to promote aqueous conversion of nitrate into volatile EtONO2. The derivative was analyzed by headspace GC–MS with 3-min elution time. The method performance was validated with a series of tests which demonstrated adequate selectivity and ruggedness. This method supported the development of novel SPIN-1 CRM giving a modest contribution to its uncertainty (uchar = 0.85%). With respect to previous attempts, the SPIN-1 was proven stable, homogeneous (uhom = 0.44%), and suitable for spinach monitoring under EU regulations. On dried basis, the nitrate content of SPIN-1 was found to be 22.53 ± 0.43 mg/g (Uc = 1.9%, k = 2). The material was also used in an inter-laboratory study where four laboratories employed a total of ten measurement methods. [ABSTRACT FROM AUTHOR]

The present study illustrates the synthesis of silver nanoparticles capped with carbon dots (AgNPs-CDs) and their application towards the sensitive and selective sensing of sulfide ions by colorimetry and spectrofluorimetry methods. The CDs were prepared from l-asparagine by pyrolysis at 234 °C. The as-synthesized CDs were then utilized as reducing and capping agents for the synthesis of AgNPs-CDs by the wet chemical method. The size of the AgNPs-CDs was found to be ~ 5.2 nm. They show a characteristic surface plasmon resonance band at 417 nm and emission maximum at 441 nm when excited at 348 nm. Since the AgNPs were formed on the surface of CDs, the emission intensity of AgNPs-CDs was drastically decreased in contrast to that of CDs. The as-synthesized AgNPs-CDs were then successfully used for the sensitive and selective determination of sulfide ions. The addition of 0.1 μM sulfide ions to AgNPs-CDs leads to a decrease in the absorbance intensity at 417 nm aside turning from yellow to colorless. In the contrary, the emission was "turned on" after the addition of sulfide ions. The decrease in the absorbance and increase in the emission were attributed to the rapid formation of Ag2S. Finally, the practical application of the present method was demonstrated by determining dissolved H2S in tap water samples. [ABSTRACT FROM AUTHOR]

A new simple, rapid and sensitive reversed-phase high-performance liquid chromatography method was developed and validated as per International Conference on Harmonization guidelines, Q2 (R1), for simultaneous estimation of isoniazid, pyrazinamide and rifampicin in solid lipid nanoparticles. Separation was achieved on a 250x4.6 mm, 5 µm, C-18 column using a linear gradient flow rate of 1.5 ml/min. Isoniazid, pyrazinamide and rifampicin were identified based on their retention times as compared to standards and confirmed with characteristic spectra on a spectrophotometer at 238 nm and eluted at 3.787, 4.173 and 11.273 min, respectively, achieved within 20 min. This method was linear, precise with % RSD values of 0.18 % for isoniazid, 0.15 % for pyrazinamide and 0.47 % for rifampicin, accurate with mean recovery yields of 101.312 % for isoniazid, 99.910 % for pyrazinamide and 99.767 % for rifampicin and selective over the concentration range of 10-150 % for all the three drugs. This method is suitable due to its simplicity and accuracy for routine quality control and stability analysis of antitubercular drugs-loaded solid lipid nanoparticles. [ABSTRACT FROM AUTHOR]

This article aims to provide an overview on the transition from earlier laboratory automation using analytical flow approaches toward today’s applications of flow methodologies, recent developments, and future trends. The article is directed to flow practitioners while serving as a valuable reference to newcomers in the field in providing insight into flow techniques and conceptual differences in operation across the distinct flow generations. In the focus are the recently developed and complementary techniques Lab-On-Valve and Lab-In-Syringe. In the following, a brief comparison of the different application niches and contributions of flow techniques to past and modern analytical chemistry is given, including (i) the development of sample pretreatment approaches, (ii) the potential applicability for in-situ/on-site monitoring of environmental compartments or technical processes, (iii) the ability of miniaturization of laboratory chemistry, (iv) the unique advantages for implementation of kinetic assays, and finally (v) the beneficial online coupling with scanning or separation analytical techniques. We also give a critical comparison to alternative approaches for automation based on autosamplers and robotic systems. Finally, an outlook on future applications and developments including 3D prototyping and specific needs for further improvements is given.ᅟ [ABSTRACT FROM AUTHOR]

An optical sensor for detection of herbicides was developed through the functionalization of CdTe quantum dots (CdTe-QDs) with cysteamine hydrochloride. The functionalized CdTe-QDs was characterized with various physicochemical methods such as X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy, energy dispersive X-ray analysis, Ultraviolet-visible and photoluminescence spectroscopies. The optical band gap of the functionalized CdTe-QDs as calculated by using Tauc plot was 3.75 eV. It was found that the fluorescence intensity of the functionalized CdTe-QDs quenched linearly in the presence of different herbicides according to the Stern-Volmer equation. Thus, the functionalized CdTe-QDs can be used as simple, rapid, inexpensive, and optical sensitive sensor for practical detection of herbicides. [ABSTRACT FROM AUTHOR]

A novel and sensitive method based on nitrogen-doped carbon quantum dots as a fluorescence probe coupled with magnetic solid-phase extraction (MSPE) purification for analysis of folic acid (FA) in human serum samples has been established for the first time. In the developed system, magnetic nanoparticles coated with hexanoic acid (FeO@C) were synthesized by a one-step chemical co-precipitation method with good magnetic properties and dispersibility for sample purification, and it is better to be separated from the sample. High fluorescence nitrogen-doped carbon quantum dots (N-CQDs), simply prepared using a one-step hydrothermal method with nitrilotriacetic acid, could be selectively quenched by FA. Based on this phenomenon, a fluorescence assay was proposed for specific determination of FA. Various operational experiment parameters have been studied and optimized in detail. Under the optimum experimental conditions, the detection limit of the proposed method for FA was evaluated to be 0.5 nM (S/ N = 3), while the relative standard deviation (RSD) was 1.2% ( n = 6). Finally, the proposed method was applied for determination of trace levels of FA from human serum samples and quantitative recoveries were achieved within the range of 95.7-103.5%. All of the results showed that the proposed method had significant application in further research. [ABSTRACT FROM AUTHOR]

The present work reports a straightforward one-step synthetic route assisted by microwave irradiation for the aqueous preparation of highly luminescence CdTe quantum dots capped with different ligands, namely, 3-mercaptopropionic acid (MPA), l-glutathione reduced and 2-mercaptoethanesulfonate. Utilization of microwave heating instead of convective heating, prevailing in the conventional hydrothermal synthesis, allows for rapid, uniform and controlled nucleation and growth of nanoparticles. Moreover, the use of air-stable NaTeO as Te precursor enables a more user-friendly synthetic process averting the need for handling reagents in vacuum or under inert atmosphere. The experimental synthesis conditions for each capping were optimized by using a response surface methodology. The variables used for the optimization were the molar ratios of reagents and pH, and the optimization output was the highest photoluminescence quantum yield (QY). The optimal settings were determined by using a central composite design comprising a complete 2-factorial design as cubic points, with six axial points at a distance of α = 1.682 from the design center and four center points. Additionally, the influence of the microwave irradiation time (2-90 min) and the reaction temperature (85-150 °C) on the nanoparticles growth kinetics were thoroughly investigated. Under the optimized synthetic conditions highly luminescent (QY values up to approximately 60%), crystalline and monodisperse CdTe quantum dots with suitable surface functionalities were successfully obtained. The surface passivation with the respective capping ligand was characterized by FT-IR while the size and the high crystallinity of the as-prepared nanocrystals were confirmed by HR-TEM. [ABSTRACT FROM AUTHOR]

To design a useful lipid drug carrier having a high encapsulation efficiency ( EE%) for the antiprostate cancer drugs flutamide (FT) and nilutamide (NT), a lipid nano-emulsion (LNE) was prepared with soybean oil (SO), phosphatidylcholine (PC), and sodium palmitate, and the partition coefficients ( K s) of the drugs for the LNE were determined by F nuclear magnetic resonance (NMR) spectrometry. The F NMR signal of the trifluoromethyl group of both drugs showed a downfield shift from an internal standard (trifluoroethanol) and broadening according to the increase in the lipid concentration due to their interaction with LNE particles. The difference in the chemical shift (Δ δ) of each drug caused by the addition of LNE was measured under different amounts of LNE, and the K values were calculated from the Δ δ values. The results showed that FT has higher lipophilicity than NT. The total lipid concentration (SO + PC) required to encapsulate each drug into LNE with an EE% of more than 95% was calculated from the K values as 93.3 and 189.9 mmol/L for FT and NT, respectively. For an LNE prepared with the total lipid concentration of 215 mmol/L, the predicted EE% values were 98 and 96% for FT and NT, respectively, while the experimental EE% values determined by a centrifugation method were approximately 99% for both drugs. Thus, the F NMR spectrometric method is a useful technique to obtain the K values of fluorinated drugs and thereby predict the theoretical lipid concentrations and prepare LNEs with high EE% values. [ABSTRACT FROM AUTHOR]

In this work, a total flow analysis system based on a novel solid-liquid extraction chamber is presented. This strategy enables all the main experimental procedures for the analysis of a solid sample to be performed automatically: enrichment of the liquid extract, sample treatment, filtration of the liquid extract from the solid sample, directing the extract towards detection, and finally cleansing of the chamber for the following solid sample to be analyzed. The chamber designed to be incorporated in the flow manifold presents two main features: it accommodates stirring bars for enhancing the extraction process, and it presents replaceable solid sample containers (a spare part of the solid-liquid extraction chamber) to easily replace the solid sample and therefore enhance sample analysis throughput. The chamber performance was assessed using two different solid samples, an ion exchanger resin and vegetable samples, focussing on proton and nitrate ion extraction, respectively. The main figures of merit achieved were relative standard deviation (RSD) and relative error values below 7 % for all determinations. The determination rate for vegetable samples was ca. 12 samples h. The proposed strategy may be exploited to perform automatically the analysis of solid samples as it embodies a simple automatic strategy of a very important but time-consuming and laborious analytical operation. [ABSTRACT FROM AUTHOR]

Herein, we synthesized and characterized glutathione-capped copper nanoclusters (CuNCs) using a convenient one-pot chemical reduction approach based on glutathione as capping and reducing agents. The Ce(III) induced aggregation-induced emission of CuNCs to form a CuNCs-Ce 3+ fluoroprobe due to electrostatic and coordination interactions between Ce 3+ and CuNCs. In contrast to CuNCs, the fluorescent intensities (FLs) of CuNCs-Ce 3+ were enhanced by ~ 40-fold concomitant with 20-nm blue-shift of the maximum emission, and a 3.45-fold lengthening of the average fluorescent lifetime. The FLs of CuNCs-Ce 3+ were selectively quenched at 650 nm by hydrogen peroxide (H 2 O 2 ) via the redox reaction. Based on this phenomenon, the sensitive assay of H 2 O 2 was realized, and the linear range spanned over the range of 14-140 μM. Notably, the visualization of the fluorescence quenched effect of H 2 O 2 could be easily attained. Additionally, glucose could be specifically oxidized by glucose oxidase to produce H 2 O 2 , and thus the detection of glucose was achieved according to changes in the concentrations of H 2 O 2 . Under optimized conditions, the fluorescent assay of glucose based on the CuNCs-Ce 3+ system offered the linear range of 8-48 μM with detection limit of 2.4 μM. Meanwhile, high selectivity of the as-constructed fluorescent assay allows the sensitive detection of H 2 O 2 and glucose in real-world care products and human serum samples, showing a great application potential in their conventional monitoring.

A new approach for the implementation of liquid-liquid extraction in a sequential injection manifold is presented. The manifold consists of two syringe pumps and one multi-position valve. The use of a 30 % MeOH/HO (v/v) solution as the carrier, with isobutanol as the extractant, made it possible to avoid the problems associated with the different affinities of the organic and aqueous phases for Teflon tubing, and the formation of bubbles. The suitability of the proposed method was demonstrated by the determination of thiamine in pharmaceutical preparations and dietary supplements. Detection and quantification limits were estimated as 9 and 30 μg L, respectively. The repeatability was lower than 3 % and the intermediate precision (3 d) was lower than 7 %. The sample throughput was 14 samples per h. The results were in agreement with a high-performance liquid chromatography-electrospray/mass spectrometry reference method. [ABSTRACT FROM AUTHOR]

A capillary electrophoresis method was used for assay of some degradation products of carvedilol. The optimized parameters were as; running buffer 80 mM acetate dissolved in methanol/ethanol mixture (65:35% v/v), applied voltage of 19 kV, temperature is 20 °C and the wavelength range of 200-350 nm. The results indicate that the proposed capillary electrophoresis method could effectively separate carvedilol from its degradation products and can be employed as a stability indicating assay method. In addition, the presence of a new unknown degradation product was discovered by this method. In addition, capillary electrophoresis behaviour of carvedilol in photo/force degradation conditions gave valuable information concerning the dissimilarities of their ionization. Results indicated that the proposed method can be used for the determination of carvedilol in human serum. Finally, accuracy of the proposed method was established by recovery experiments from spiked human serum samples. [ABSTRACT FROM AUTHOR]

A fully automated method for the determination of chromate is described. It is based on the selective reaction of Cr(VI) with diphenylcarbazide in acidic media to form a colored complex of Cr(III) with the oxidation product diphenylcarbazone. The reaction was performed within the syringe of an automatic burette containing a magnetic stirrer for homogenization of the sample and the required reagents. In-syringe stirring was made possible using a specially designed driving device placed around the syringe barrel to achieve a rotating magnetic field in the syringe, forcing the stirrer to spin. In a second step, the reaction mixture in the syringe was neutralized to allow in-syringe magnetic-stirring-assisted dispersive liquid-liquid microextraction of the complex into 125 μL of n-hexanol. After phase separation by droplet flotation over 30 s, the organic phase was propelled into a coupled spectrophotometric detection cell. The entire multistep procedure including in-system standard preparation was done within 270 s. The method was used for the analysis of natural waters, achieving average analyte recovery of 103 %, a limit of detection of 0.26 μg L, and a repeatability of less than 4 % relative standard deviation. [ABSTRACT FROM AUTHOR]

A simple and fast electroanalytical method for the detection of nitrate at an in situ copper-modified glassy carbon electrode (GCE) in an acidic media is proposed on the basis of square wave voltammetry. Since the fresh copper-modified electrode was formed in situ and the signals of nitrate were recorded in time, the whole experiment does not require sample preparation and oxygen removal from the solution degassed with nitrogen. Finally, a procedure for on-line electrochemical cleaning, the surface of GCE was employed to keep the copper film fresh. The whole experiment was rapid, in no more than 10 min. Under the optimal conditions, nitrates could be quantitatively determined in the range extending from 10 to 300 μM, a very good linear correlation ( R = 0.9996) can be observed when analyzing the relationship between the peak current and the ion concentration. In addition, the interferential effects of some common anions in water samples on the nitrate determination were also investigated. The results show that only nitrite ions could produce a distinct peak current at the same potential as nitrate does. When applying this method to detect nitrate in real water samples, the results exhibit good sensitivity. The procedure was also verified by the standard optical method. [ABSTRACT FROM AUTHOR]

A multisyringe flow-injection approach has been coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) with UV photo-oxidation for dimethylarsinic (DMA), inorganic As and total As determination, depending on the pre-treatment given to the sample (extraction or digestion). The implementation of a UV lamp allows on-line photo-oxidation of DMA and the following arsenic detection, whereas a bypass leads the flow directly to the HG-AFS system, performing inorganic arsenic determination. DMA concentration is calculated by the difference of total inorganic arsenic and measurement of the photo-oxidation step. The detection limits for DMA and inorganic arsenic were 0.09 and 0.47 μg L, respectively. The repeatability values accomplished were of 2.4 and 1.8 %, whereas the injection frequencies were 24 and 28 injections per hour for DMA and inorganic arsenic, respectively. This method was validated by means of a solid reference material BCR-627 (muscle of tuna) with good agreement with the certified values. Satisfactory results for DMA and inorganic arsenic determination were obtained in several water matrices. The proposed method offers several advantages, such as increasing the sampling frequency, low detection limits and decreasing reagents and sample consumption, which leads to lower waste generation. [ABSTRACT FROM AUTHOR]

A new approach for the integration of various analytical steps inside a syringe (Lab in a Syringe) is presented. Fully automated dispersive liquid-liquid microextraction with integrated spectrophotometric detection is carried out in-syringe using a very simple instrumental setup. The lighter-than-water organic droplets released in the extraction step accumulate at the head of the syringe, where two optical fibers are placed on both sides of the syringe, facing each other and enabling the in situ quantification of the extracted compounds. By this, monitoring of the progressively accumulating droplet in the head of the syringe was further possible. In this first report, the developed instrumental setup has been applied to the determination of the dye rhodamine B in water samples and soft drinks. The main parameters influencing the extraction such as the selection of the extractant and disperser solvents, extractant/disperser and organic/water phase ratios, pH of the aqueous phase, extraction flow rates, and extraction time were investigated. Under the selected conditions, rhodamine B was quantified in a working range of 0.023-2 mg L with a limit of detection of 0.007 mg L. Good repeatability values of up to 3.2 % (RSD) were obtained for ten consecutive extractions. The enrichment factor for a 1 mg L rhodamine B standard was 23, and up to 51 extractions were accomplished in 1 h. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

We report herein a novel chemiluminescence (CL) phenomenon triggered by light irradiation when a fluorescent dye, for example hematoporphyrin, fluorescein, eosin, or methylene blue is present in the luminol solution. A possible mechanism is proposed for the photoinduced chemiluminescence (PICL) reaction. Compared with reported methods for CL triggering, for example flow-injection, static reagent injection, and the electrochemical technique, the proposed in-situ PICL method presented has three advantages. First, the method is more selective, because the PICL signal of the target fluorescent dyes is initiated by excitation at a selective wavelength only. Second, the space and time resolution of the PICL method are better. Last, and most important, compared with injecting a reagent or inserting a electrode into the CL system to initiate the CL reaction, with the in-situ PICL method there is no physical interference with the target detecting system. All these advantages of the PICL method indicate it has many potential applications in the analytical sciences. The proposed method was applied to analysis of urine containing adrenaline. The linear range for adrenaline is 2.0 × 10-1.0 × 10 g mL and the detection limit is 6.0 × 10 g mL. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

We have examined a range of new and previously described flow cells for chemiluminescence detection. The reactions of acidic potassium permanganate with morphine and amoxicillin were used as model systems representing the many fast chemiluminescence reactions between oxidising agents and organic analytes, and the preliminary partial reduction of the reagent was exploited to further increase the rates of reaction. The comparison was then extended to high-performance liquid chromatography separations of α- and β-adrenergic agonists, with permanganate chemiluminescence detection. Flow cells constructed by machining novel channel designs into white polymer materials (sealed with transparent films or plates) have enabled improvements in mixing efficiency and overall transmission of light to the photodetector. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

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new procedure for spectrofluorimetric determination of free and total glycerol in biodiesel samples is presented. It is based on the oxidation of glycerol by periodate, forming formaldehyde, which reacts with acetylacetone, producing the luminescent 3,5-diacetyl-1,4-dihydrolutidine. A flow system with solenoid micro-pumps is proposed for solution handling. Free glycerol was extracted off-line from biodiesel samples with water, and total glycerol was converted to free glycerol by saponification with sodium ethylate under sonication. For free glycerol, a linear response was observed from 5 to 70 mg L with a detection limit of 0.5 mg L, which corresponds to 2 mg kg in biodiesel. The coefficient of variation was 0.9% (20 mg L, n = 10). For total glycerol, samples were diluted on-line, and the linear response range was 25 to 300 mg L. The detection limit was 1.4 mg L (2.8 mg kg in biodiesel) with a coefficient of variation of 1.4% (200 mg L, n = 10). The sampling rate was ca. 35 samples h and the procedure was applied to determination of free and total glycerol in biodiesel samples from soybean, cottonseed, and castor beans. [ABSTRACT FROM AUTHOR]

rapid and simple miniaturized liquid-liquid extraction method has been developed for the determination of topramezone in soil, corn, wheat, and water samples using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-electrospray ionization (ESI)/MS/MS). The established method for the extraction and purification procedure was based on liquid-liquid partitioning into an aqueous solution at a low pH (pH ≈ 2.5), followed by back-partitioning into water at pH > 9. Two precursor, product ion transitions for topramezone were measured and evaluated to provide the maximum degree of confidence in the results. Under negative ESI conditions, quantitation was achieved by monitoring the fragment at m/ z = 334 and the qualitative fragment at m/ z = 318, whereas also collecting the corresponding parent ion at m/ z = 362. Chromatographic separation was achieved using gradient elution with a mobile phase consisting of methanol and a 0.01% aqueous ammonium hydroxide solution. Recovery studies for soil, corn, wheat, and water were conducted at four different topramezone concentrations (5 or 10, 50, 100, and 1,000 μg kg); the overall average recoveries ranged from 79.9% to 98.4% with intra-day relative standard deviations (RSD) of 3.1~8.7% and inter-day RSD of 4.3~7.5%. Quantitative results were determined from calibration curves of topramezone standards containing 1-500 μg L with an R ≥ 0.9994. Method sensitivities expressed as limits of quantitation were typically 6, 8, 9, and 1 μg kg in soil, corn, wheat, and water, respectively. The results of the method validation confirmed that this proposed method was convenient and reliable for the determination of topramezone residues in soil, corn, wheat, and water. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

A simple spectrophotometric method was developed for the analysis of inulin in Jerusalem artichoke tubers. The inulin was extracted from the artichoke tuber samples using accelerated solvent extraction method, before subsequent hydrolysis in acid condition. The hydrolysates were then analyzed for fructose using spectrophotometry. The spectrophotometric method is based on oxidation of fructose by periodate and evaluation of the remaining periodate by measuring the absorbance at 350 nm of the tri-iodide complex formed, upon addition of potassium iodide. The optimum conditions for the detection of fructose were 0.1 mmol L periodate and 1.5 mmol L potassium iodide at pH 6.0. The proposed method was validated for its analytical performance parameters including accuracy, precision, and recovery. The method was applied to the determination of inulin in ten varieties of Jerusalem artichoke grown in the northeastern part of Thailand. The inulin content in the samples was found to be in the range of 63-75.5% dry weight, and the degree of polymerization was in the range of 14-20. The inulin contents obtained from the proposed spectrophotometry were not significantly different ( p = 0.05) from those obtained from high-performance anion-exchange chromatography coupled with pulsed amperometric detection. The results indicated that the present spectrophotometric method can be used as an alternative to chromatographic analysis for the determination of inulin in plant samples. [ABSTRACT FROM AUTHOR]