Determination of cyanide in urine and saliva samples by ion chromatography with pulsed amperometric detection.
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ABSTRACT:
SUBMITTER: Jaszczak E
PROVIDER: S-EPMC5541122 | biostudies-other | 2017
REPOSITORIES: biostudies-other
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Project description:Chinese medicine residues contain abundant cellulose and hemicellulose, which are potential renewable carbon sources for ethanol production. The aim of the present study was to develop a rapid and reliable method to evaluate the cellulose and hemicellulose utilization in Chinese medicine residues. In the present study, key hydrolysates (arabinose, galactose, glucose, xylose, and cellobiose) of the cellulose and hemicellulose in fermentation liquor of Astragalus residues were simultaneously quantified by ion chromatography using an integrated pulsed amperometric detector (IPAD). HPLC analysis was performed on a Dionex ICS-2500 equipped with GP50 gradient pump and ED50 IPAD. The working and reference electrodes were gold electrode and Ag/AgCl electrode, respectively. Separation was achieved on serial no. 002627 Dionex Analytical column (2×250 mm). Sodium hydroxide of 250 mM and water were used as the mobile phase with a flow rate of 0.2 ml/min. The temperature of column was kept at 30°C. This method was validated for accuracy and precision. The regression equation revealed a good linear relationship (R2=0.9959-0.9984) within the test ranges. The limits of detection and quantification for five standard analytes (arabinose, galactose, glucose, xylose and cellobiose) were in the range of 0.067-0.091 and 0.08-0.23 mg/l, respectively. The method showed good reproducibility for the quantification of five analytes in fermentation liquor of Astragalus residue with intra-and inter-day variations less than 3.843%.
| S-EPMC5525577 | biostudies-other
Project description:Nitrite is considered an important target analyte for environmental monitoring. In water resources, nitrite is the result of the nitrogen cycle and the leaching processes of pesticides based on nitrogenous compounds. A high concentration of nitrite can be associated with intoxication processes and metabolic disorders in humans. The present study describes the development of a portable analytical methodology based on microchip electrophoresis coupled with amperometric detection for the determination of nitrite in environmental water samples. Electrophoretic and detection conditions were optimized, and the best separations were achieved within 60 s by employing a mixture of 30 mmol L-1 lactic acid and 15 mmol L-1 histidine (pH = 3.8) as a running buffer applying 0.7 V to the working electrode (versus Pt) for amperometric measurements. The developed methodology revealed a satisfactory linear behavior in the concentration range between 20 and 80 μmolL-1 (R2 = 0.999) with a limit of detection of 1.3 μmolL-1. The nitrite concentration was determined in five water samples and the achieved values ranged from (28.7 ± 1.6) to (67.1 ± 0.5) µmol L-1. The data showed that using the proposed methodology revealed satisfactory recovery values (83.5-103.8%) and is in good agreement with the reference technique. Due to its low sample consumption, portability potential, high analytical frequency, and instrumental simplicity, the developed methodology may be considered a promising strategy to monitor and quantitatively determine nitrite in environmental samples.
| S-EPMC9610075 | biostudies-literature
Project description:BackgroundCurrent detection or screening for malaria infection necessitates drawing blood by fingerprick or venipuncture, which poses risks and limitations for repeated measurement. This study presents PCR detection of Plasmodium falciparum in human urine and saliva samples, and illustrates this potential application in genotyping malaria infections.MethodsUrine and saliva were obtained from 47 thick film positive and 4 negative individuals one day after collection of blood slides and filter paper blood spots. P. falciparum DNA was extracted from blood, urine and saliva, in separate groups, using the Chelex method or Qiagen DNEasy kit (urine and saliva only). Blood, urine and saliva extracts were subjected to PCR in separate batches. Amplicons from the various sample types were examined for MSP2 polymorphisms and restriction fragment patterns on DHFR amino acid codon 59.Results and discussionMalaria infections exhibited primarily low-grade parasite densities, with a geometric mean of 775 asexual parasites/mul. Regularly matching polymorphic MSP2 genotypes were found between the corresponding urine, saliva and peripheral blood amplicons of each individual, with different inter-individual polymorphic genotypes. Amplicon yields were significantly dependent on DNA extraction method, parasite density and primer set (p < 0.001). A Qiagen kit extraction had more than 2x higher amplicon yield than the Chelex method, for both urine and saliva. Amplicon yields were 1.6 fold higher from saliva than urine. For each unit increase in log parasite density, the probability of amplicon enhanced 1.8 fold. Highest amplicon yields were obtained from the primer set with the shortest PCR product.ConclusionP. falciparum infection is detectable by PCR on human urine and saliva samples. Subject to further refinement of extraction technique and amplicon yields, large-scale malaria parasite screening and epidemiological surveys could be possible without the need to collect blood and use of needles or sharps.
| S-EPMC1654175 | biostudies-literature
Project description:We have designed and synthesized a novel simple colorimetric fluorescent probe with aggregation-induced emission (AIE) properties. Probe 5-(4-(diphenylamine)phenyl) thiophen-2-formaldehyde W exhibited a turn-on fluorescent response to cyanide ion (CN−), which induces distinct visual color changes. Probe W exhibited a highly selective and sensitive ratiometric fluorescence response for the detection of CN− over a wide pH range (4–11) and in the presence of common interferents. The linear detection of CN− over the concentration range of 4.00–38.00 µM (R2 = 0.9916, RSD = 0.02) was monitored by UV-Vis absorption spectrometry (UV-Vis) with the limit of detection determined to be 0.48 µM. The linear detection of CN− over the concentration range of 8.00–38.00 µM was examined by fluorescence spectrophotometry (R2 = 0.99086, RSD = 0.031), and the detection limit was found to be 68.00 nM. The sensing mechanisms were confirmed by 1H NMR spectroscopic titrations, X-ray crystallographic analysis, and HRMS. Importantly, probe W was found to show rapid response, high selectivity, and sensitivity for cyanide anions in real water samples, over the range of 100.17∼100.86% in artificial lake water and 100.54∼101.64% in running water by UV-Vis absorption spectrometry, and over the range of 99.42∼100.71% in artificial lake water and 100.59∼101.17% in running water by fluorescence spectrophotometry. Importantly, this work provides a simple and effective approach which uses an economically cheap and uncomplicated synthetic route for the selective, sensitive, and quantitative detection of CN− ions in systems relevant to the environment and health.
| S-EPMC9339681 | biostudies-literature
Project description:BackgroundWhite ginseng consists of the roots and rhizomes of the Panax species, and red ginseng is made by steaming and drying white ginseng. While red ginseng has both polar and nonpolar ginsenosides, previous studies showed white ginseng to have only polar ginsenosides. Because nonpolar ginsenosides are formed through the manufacture of red ginseng from white ginseng, researchers have generally thought that nonpolar ginsenosides do not exist in white ginseng.MethodsWe developed a simultaneous quantitative method for six nonpolar ginsenosides in white ginseng using reverse-phase high-performance liquid chromatography coupled with integrated pulsed amperometric detection. The nonpolar ginsenosides of white ginseng were extracted for 4 h under reflux with 50% methanol.ResultsUsing the gradient elution system, all target components were completely separated within 50 min. Nonpolar ginsenosides were determined in the rhizome head (RH), main root (MR), lateral root, and hairy root (HR) of 6-year-old white ginseng samples obtained from several regions (Geumsan, Punggi, and Kanghwa). The total content in the HR of white ginseng was 37.8-56.8% of that in the HR of red ginseng. The total content in the MR of white ginseng was 5.9-24.3% of that in the MR of red ginseng. In addition, the total content in the RH of white ginseng was 28.5-35.8% of that in the HR of red ginseng.ConclusionIt was confirmed that nonpolar ginsenosides known to be specific components of red ginseng were present at substantial concentrations in the HR or RH of white ginseng.
| S-EPMC7322751 | biostudies-literature
Project description:Oropouche virus (OROV) is an arthropod-borne virus of the Peribunyaviridae family, transmitted to humans primarily by Culicoides paraensis. It is one of the main arboviruses infecting humans in Brazil, primarily in the Amazon Region. Here, we report the detection of OROV in the saliva and urine of a patient whose samples were collected five days after the onset of symptoms. Nucleotide sequencing and phylogenetic analysis further confirmed the results. To our knowledge, this is the first study reporting the detection of OROV in the saliva and urine of an infected patient. In addition, the results of our study expand the current knowledge pertaining to the natural history of Oropouche fever.
| S-EPMC7046135 | biostudies-literature
Project description:BackgroundSaliva sampling is one of the methods of therapeutic drug monitoring for mycophenolic acid (MPA) and its metabolite, mycophenolic acid glucuronide (MPAG). The study describes the liquid chromatography tandem mass spectrometry (LC-MS/MS) method developed for saliva MPA and MPAG determination in children with nephrotic syndrome.MethodsThe mobile phase consisted of methanol and water at gradient flow, both with 0.1% formic acid. Firstly, 100 µL of saliva was evaporated at 45 °C for 2 h to dryness, secondly, it was reconstituted in the mobile phase, and finally 10 µL was injected into the LC-MS/MS system. Saliva from ten children with nephrotic syndrome treated with mycophenolate mofetil was collected with Salivette®.ResultsFor MPA and MPAG, within the 2-500 ng/mL range, the method was selective, specific, accurate and precise within-run and between-run. No carry-over and matrix effects were observed. Stability tests showed that MPA and MPAG were stable in saliva samples if stored for 2 h at room temperature, 18 h at 4 °C, and at least 5 months at - 80 °C as well as after three freeze-thaw cycles, in a dry extract for 16 h at 4 °C, and for 8 h at 15 °C in the autosampler. The analytes were not adsorbed onto Salivette® cotton swabs. For concentrations above 500 ng/mL, the samples may be diluted twofold. In children, saliva MPA and MPAG were within the ranges of 4.6-531.8 ng/mL and 10.7-183.7 ng/mL, respectively.ConclusionsThe evaluated LC-MS/MS method has met the validation requirements for saliva MPA and MPAG determination in children with nephrotic syndrome. Further studies are needed to explore plasma-saliva correlations and assess their potential contribution to MPA monitoring.
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Project description:The emergence of a new class of novel psychoactive substances, N-benzyl-substituted phenethylamine derivatives so-called "NBOMes" or "Smiles", in the recreational drug market has forced the development of new sensitive analytical methodologies for their detection and quantitation. NBOMes' hallucinogenic effects mimic those of the illegal psychedelic drug lysergic acid diethylamide (LSD) and are typically sold as LSD on blotter papers, resulting in a remarkable number of fatalities worldwide. In this article, four halide derivatives of NBOMe, namely, 2-(4-fluoro-2,5-dimethoxyphenyl)-N-(2-methoxybenzyl)ethan-1-amine, 2-(4-chloro-2,5-dimethoxyphenyl)-N-(2-methoxybenzyl)ethan-1-amine, 2-(4-bromo-2,5-dimethoxyphenyl)-N-(2-methoxybenzyl)ethan-1-amine, and 2-(4-iodo-2,5-dimethoxyphenyl)-N-(2-methoxybenzyl)ethan-1-amine, were detected and quantified simultaneously using a high-performance liquid chromatographic method, and two detection systems were compared: photodiode array detection (detection system I) and amperometric detection via a commercially available impinging jet flow-cell system incorporating embedded graphite screen-printed macroelectrodes (detection system II). Under optimized experimental conditions, linear calibration plots were obtained in the concentration range of 10-300 and 20-300 ?g mL-1, for detection systems I and II, respectively. Detection limit (limit of detection) values were between 4.6-6.7 and 9.7-18 ?g mL-1, for detection systems I and II, respectively. Both detectors were employed for the analysis of the four NBOMe derivatives in the bulk form, in the presence of LSD and adulterants commonly found in street samples (e.g. paracetamol, caffeine, and benzocaine). Furthermore, the method was applied for the analysis of simulated blotter papers, and the obtained percentage recoveries were satisfactory, emphasizing its advantageous applicability for the routine analysis of NBOMes in forensic laboratories.
| S-EPMC6740171 | biostudies-literature
Project description:A rapid, accurate, and sensitive analytical method, ultrasonication-assisted spraying based fine droplet formation-liquid phase microextraction-gas chromatography-mass spectrometry (UA-SFDF-LPME-GC-MS), was proposed for the determination of trace amounts of hydroxychloroquine sulfate in human serum, urine, and saliva samples. To determine the best extraction strategy, several liquid and solid phase extraction methods were investigated for their efficiencies in isolation and preconcentration of hydroxychloroquine sulfate from biological matrices. The UA-SFDF-LPME method was determined to be the best extraction method as it was operationally simple and provided accurate results. Variables such as the extraction solvent, spraying number, sodium hydroxide concentration and volume, sample volume, mixing method, and mixing period were optimized for the proposed method using the one-variable-at-a-time approach. In addition, Tukey's method based on a post hoc comparison test was employed to evaluate the significant difference between the parameters inspected. After the optimization studies, the limit of detection (LOD) and limit of quantification (LOQ) were determined to be 0.7 and 2.4 μg/kg, respectively. The sensitivity of the GC-MS system based on the LOD was enhanced approximately 440-fold when the UA-SFDF-LPME method was employed. Spiking experiments were also conducted for the human serum, urine, and saliva samples to determine the applicability and accuracy of the proposed method. Recoveries for the human serum, urine, and saliva samples were found to be in the ranges of 93.9%-101.7%, 95.2%-105.0%, and 93.1%-102.3%, respectively. These results were satisfactory and indicated that the hydroxychloroquine sulfate level in the above biological samples could be analyzed using the proposed method.
| S-EPMC7847195 | biostudies-literature
Project description:High-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) combined with chemometric analysis was developed to describe, for the first time, the sugar profile of sixty-one honeys of different botanical origin produced in southern Italy (Calabria Region). The principal component and linear discriminant analysis used to describe the variability of sugar data were able to discriminate the honeys according to their botanical origin with a correlation index higher than 90%. For the purpose of the robustness of the conclusions of this study, the analytical advantages of the HPAEC-PAD method have been statistically demonstrated compared to the official Italian HPLC-RI method (Refractive Index detection). Finally, as the characterization of the floral and geographical origin of honey became an important issue due to high consumer demand, 13 acacia honeys originating from Europe and China were studied by using the same method. By chemometric method it was possible to discriminate the different geographical origin with an index of 100%. All results proved the possibility to identify the sugar profile obtained by HPAEC-PAD combined with a robust statistical analysis, as a tool of authentication.
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