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Sewage-based epidemiology in monitoring the use of new psychoactive substances: Validation and application of an analytical method using LC-MS/MS

机译:基于污水的流行病学监测新型精神活性物质的使用:使用LC-MS / MS的分析方法的验证和应用

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Sewage-based epidemiology (SBE) employs the analysis of sewage to detect and quantify drug use within a community. While SBE has been applied repeatedly for the estimation of classical illicit drugs, only few studies investigated new psychoactive substances (NPS). These compounds mimic effects of illicit drugs by introducing slight modifications to chemical structures of controlled illicit drugs. We describe the optimization, validation, and application of an analytical method using liquid chromatography coupled to positive electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seven NPS in sewage: methoxetamine (MXE), butylone, ethylone, methylone, methiopropamine (MPA), 4-methoxymethamphetamine (PMMA), and 4-methoxyamphetamine (PMA). Sample preparation was performed using solid-phase extraction (SPE) with Oasis MCX cartridges. The LC separation was done with a HILIC (150 x 3mm, 5 mu m) column which ensured good resolution of the analytes with a total run time of 19min. The lower limit of quantification (LLOQ) was between 0.5 and 5ng/L for all compounds. The method was validated by evaluating the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recoveries and matrix effects. The method was applied on sewage samples collected from sewage treatment plants in Belgium and Switzerland in which all investigated compounds were detected, except MPA and PMA. Furthermore, a consistent presence of MXE has been observed in most of the sewage samples at levels higher than LLOQ. Copyright (c) 2015 John Wiley & Sons, Ltd.
机译:基于污水的流行病学(SBE)利用对污水的分析来检测和量化社区内的毒品使用情况。虽然SBE已被反复用于经典违禁药物的评估,但只有很少的研究调查了新的精神活性物质(NPS)。这些化合物通过对受控非法药物的化学结构进行轻微修饰来模仿非法药物的作用。我们描述了液相色谱与电喷雾串联质谱(LC-ESI-MS / MS)联用的分析方法的优化,验证和应用,用于测定污水中的7种NPS:甲氧西敏(MXE),丁酮,甲酮,甲硫基丙胺(MPA),4-甲氧基甲基苯丙胺(PMMA)和4-甲氧基苯丙胺(PMA)。使用固相萃取(SPE)和Oasis MCX小柱进行样品制备。 LC分离使用HILIC(150 x 3mm,5μm)色谱柱完成,该色谱柱可确保分析物具有良好的分离度,总运行时间为19分钟。所有化合物的定量下限(LLOQ)在0.5和5ng / L之间。通过评估以下参数验证了该方法的有效性:灵敏度,选择性,线性,准确性,精密度,回收率和基质效应。该方法适用于从比利时和瑞士的污水处理厂收集的污水样品,在这些样品中检测到了所有被调查的化合物,MPA和PMA除外。此外,在大多数污水样品中均观察到MXE的含量始终高于LLOQ。版权所有(c)2015 John Wiley&Sons,Ltd.

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