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UHPLC-MS/MS method for simultaneously detecting 16 tryptamines and their metabolites in human hair and applications to real forensics cases
Journal of Chromatography B ( IF 3 ) Pub Date : 2020-10-16 , DOI: 10.1016/j.jchromb.2020.122392
Yan Shi , Roujia Wang , Shuai Yuan , Huosheng Qiang , Min Shen , Baohua Shen , Olaf H. Drummer , Zhiguo Yu , Yunli Zhao , Ping Xiang

Tryptamines are hallucinogenic substances many of which have appeared recently as novel psychoactive substances (NPS). Herein, we describe the establishment of a rapid UHPLC-MS/MS quantitative method for the targeted screening of 16 tryptamines of abuse in hair. Twenty milligram pieces of hair were pulverized below 4 °C in 0.5 mL of deionized water containing 0.1% formic acid and an internal standard (2 ng/mL psilocin-d10 and psilocybin-d4). After subsequent centrifugation, 5 μL of the supernatant was injected into a LC–MS/MS system fitted with a Waters Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 mm). The column was gradient eluted at 0.3 mL/min with mobile phases composed of 20 mmol/L ammonium acetate, 5% acetonitrile, and 0.1% formic acid in water (solvent A) and acetonitrile (solvent B). Limits of detection ranged between 0.1 and 20 pg/mg, with limits of quantitation ranging from 3 to 50 pg/mg. The calibration curves for all analytes were linear (r >0.992). Accuracies varied between 91% and 114%, with intraday precision RSDs < 14% and interday precision RSDs of between 1.3% and 14%. The recoveries of all tryptamines were in the 85–115% range, with the matrix effect ranging from 95% to 112%. The validated method was successfully used to analyse 191 hair samples from suspected tryptamine users, 77 of which were 5-MeO-DiPT-positive, while the 16 tryptamines and their metabolites were not detected in the remaining 114 hair samples. 5-MeO-DiPT and its 5-MeO-NiPT, 5-OH-DiPT, and 4-OH-DiPT metabolites were concurrently detected in 34 hair samples. 5-MeO-DiPT, as the parent drug, was the parent substance found in the hair samples.



中文翻译:

UHPLC-MS / MS方法同时检测人发中的16种色胺及其代谢物及其在实际法医案例中的应用

色胺是一种致幻物质,其中许多物质最近已作为新型精神活性物质(NPS)出现。在这里,我们描述了一种快速UHPLC-MS / MS定量方法的建立,用于针对性筛选头发中16种色胺的滥用。在低于4°C的温度下,将20毫克的头发在0.5 mL的含0.1%甲酸和内标物(2 ng / mL psilocin-d 10和psilocybin-d 4)的去离子水中粉碎。在随后的离心之后,将5μL上清液注入装有Waters Acquity UPLC HSS T 3的LC–MS / MS系统中色谱柱(100毫米×2.1毫米,1.8毫米)。用0.3 mL / min的流速将色谱柱梯度洗脱,流动相由20 mmol / L乙酸铵,5%乙腈和0.1%甲酸的水溶液(溶剂A)和乙腈(溶剂B)组成。检测限为0.1至20 pg / mg,定量限为3至50 pg / mg。所有分析物的校准曲线均为线性(r> 0.992)。精度在91%和114%之间变化,日内精确RSD <14%,日间精确RSD在1.3%和14%之间。所有色胺的回收率在85–115%范围内,基质效应范围从95%至112%。经过验证的方法已成功用于分析191名疑似色胺使用者的头发样本,其中77名是5-MeO-DiPT阳性,而其余114个头发样本中未检测到16种色胺及其代谢产物。在34个头发样本中同时检测到5-MeO-DiPT及其5-MeO-NiPT,5-OH-DiPT和4-OH-DiPT代谢产物。5-MeO-DiPT作为母体药物,是在头发样本中发现的母体物质。

更新日期:2020-10-17
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