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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
JPC - Journal of Planar Chromatography - Modern TLC ( IF 1.1 ) Pub Date : 2020-06-22 , DOI: 10.1007/s00764-020-00022-3
Praveen U. Sanganalmath , Purigali M. Nagaraju , Kuruba Sreeramulu

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 60F254 TLC plates using mobile phase n-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 μg/mL (0.04 to 2 μg/spot) and the sensitivity of the method (LLOQ) was 2 μg/mL (0.04 μg/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 μg/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.

中文翻译:

一种简便快速的薄层色谱-紫外光密度法测定法医学毒理学应用中人全血中三唑磷的开发与验证

尚无已发表的研究报告致命性中毒后人体全血中的三唑磷(TZP)分析。在这项研究中,描述了一种使用液-液萃取(LLE)和薄层色谱(TLC)-紫外线(UV)密度测定法测定人全血中TZP的方法。色谱法在硅胶上进行60F 254使用移动相TLC板Ñ正己烷:丙酮(8:2,V / V)和248 nm的紫外光密度检测。使用pH 5的乙酸乙酯溶剂可实现更好的萃取效果,回收率为92.17%。血液中TZP的校准曲线在2至100μg/ mL(0.04至2μg/ spot)之间呈线性关系,该方法的灵敏度(LLOQ)为2μg/ mL(0.04μg/ spot)。该方法显示出2、10和50μg/ mL的加标血样的日内精度(0.37至0.82%,RSD)和日间精度(0.39至1.47%,RSD)。在不同的存储条件下,血液中TZP的测量偏差不超过2.69%。据报道,在两例致命的中毒病例中,TZP浓度较高。据我们所知,这是第一种经过验证的薄层色谱-紫外光密度法,用于测定人全血中的TZP。
更新日期:2020-06-22
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