首页> 外文期刊>Journal of Planar Chromatography-Modern TLC: JPC >Development and validation of a simple and rapid thin-layer chromatography-UV densitometry method for the determination of triazophos in human whole blood for forensic toxicological applications
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Development and validation of a simple and rapid thin-layer chromatography-UV densitometry method for the determination of triazophos in human whole blood for forensic toxicological applications

机译:一种简单快速薄层色谱 - UV密度测定方法的开发与验证,用于测定人类全血中三唑族毒理学应用

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摘要

No published studies reported triazophos (TZP) analysis in human whole blood following fatal intoxication. In this study, a method for the determination of TZP in human whole blood using liquid-liquid extraction (LLE) and thin-layer chromatography (TLC)-ultraviolet (UV) densitometry is described. Chromatography was performed on silica gel 60F(254)TLC plates using mobile phasen-hexane:acetone (8:2,v/v) and UV densitometric detection at 248 nm. Better extractions were achieved by using ethyl acetate solvent at pH 5 with a recovery of 92.17%. Calibration curve for TZP in blood was linear from 2 to 100 mu g/mL (0.04 to 2 mu g/spot) and the sensitivity of the method (LLOQ) was 2 mu g/mL (0.04 mu g/spot). The method showed excellent within-day precision (0.37 to 0.82%, RSD) and between-day precision (0.39 to 1.47%, RSD) for spiked blood samples at 2, 10, and 50 mu g/mL. The measured concentrations of TZP in blood did not deviate more than 2.69% under different storage conditions. TZP concentrations in two fatal cases of poisoning were reported. To the best of our knowledge, this is the first validated TLC-UV densitometric method developed to determine TZP in human whole blood.
机译:没有公布的研究报告了致命中毒后人类全血中的三唑(TZP)分析。在该研究中,描述了使用液 - 液萃取(LLE)和薄层色谱(TLC)硫纤维(UV)密度测定法测定人类全血中TZP的方法。使用移动相己烷:丙酮(8:2,v / v)和248nm的丙酮(8:2,v / v)检测,在硅胶60f(254)Tlc板上进行色谱法。通过在pH5下使用乙酸乙酯溶剂来实现更好的提取,回收率为92.17%。血液中TZP的校准曲线从2至100μg/ ml(0.04至2μg/斑)的线性线性,方法(LLOQ)的敏感性为2μg/ ml(0.04μg/斑)。该方法显示出在日期内的精度优异(0.37至0.82%,RSD),在2,10和50μg/ mL时,尖刺血液样品的白天精度(0.39至1.47%,RSD)。在不同的储存条件下,血液中TZP的测量浓度不会偏离2.69%。报道了两种致命病例中的TZP浓度。据我们所知,这是第一种验证的TLC-UV密度测量方法,用于确定人类全血中的TZP。

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