Improvements in analytical methodology for the determination of frequently consumed illicit drugs in urban wastewater
Improvements in analytical methodology for the determination of frequently consumed illicit drugs in urban wastewater
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DOI：
10.1007/s00216-014-7818-4
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发表时间：
2014-07-01
影响因子：
4.3
通讯作者：
Hernandez, Felix
中科院分区：
文献类型：
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作者：
Bijlsma, Lubertus;Beltran, Eduardo;Hernandez, Felix
开发了基于超高效液相色谱-串联质谱法的快速灵敏分析方法，用于确定城市废水中广泛消费的滥用药物（安非他明、摇头丸、可卡因、类阿片、大麻和氯胺酮）及其主要代谢物。使用Oasis HLB通过通用离线SPE程序进行样品净化和预浓缩。在测试的废水样品中发现安非他明问题很大，因此特别努力将安非他明掺入其中，包括使用Oasis MCX SPE和分散伯仲胺进行额外的清理。通过使用同位素标记的内标物（ILIS）校正储存期间可能的SPE损失或降解，该内标物可用于所有化合物，并作为替代物添加到样品中。虽然ILIS也是有效的基质效应校正，观察到的强电离抑制没有消除，因此，四倍稀释前的SPE应用于进水废水和低注射体积选择（3 μ L），以达到基质效应，色谱性能和灵敏度之间的妥协。在25和200 ng L-1（流出液）以及100和800 ng L-1（流入液）下对该方法进行了验证，获得了0.4-25 ng L-1（流出液）和2-100 ng L-1（流入液）之间的定量限（即化合物可定量的最低水平，并通过至少两次MS/MS转换进行确认）。该方法的适用性证明了14个流入和14个流出的废水样品收集超过2个星期，在卡斯特林（西班牙）在欧洲合作研究的分析。
Rapid and sensitive analytical methodology based on ultra high-performance liquid chromatography-tandem mass spectrometry has been developed for the determination of widely consumed drugs of abuse (amphetamines, MDMA, cocaine, opioids, cannabis and ketamine) and their major metabolites in urban wastewaters. Sample clean-up and pre-concentration was performed by a generic off-line SPE procedure using Oasis HLB. Special effort was made to incorporate amphetamine, which was found highly problematic in the wastewater samples tested, including an additional clean-up with Oasis MCX SPE and dispersive primary secondary amine. Correction for possible SPE losses or degradation during storage was made by the use of isotope-labelled internal standards (ILIS), available for all compounds, which were added to the samples as surrogates. Although ILIS were also efficient for matrix effects correction, the strong ionization suppression observed was not eliminated; therefore, a four-fold dilution prior to SPE was applied to influent wastewaters and a low injection volume was selected (3 mu L), in order to reach a compromise between matrix effects, chromatographic performance and sensitivity. The method was validated at 25 and 200 ng L-1 (effluent), and 100 and 800 ng L-1 (influent), obtaining limits of quantification (i.e. the lowest level that the compound can be quantified and also confirmed with at least two MS/MS transitions) between 0.4-25 ng L-1 (effluent) and 2-100 ng L-1 (influent). The applicability of the method was demonstrated by analysis of 14 influent and 14 effluent wastewater samples collected over 2 weeks in Castelln (Spain) within a European collaborative study.