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用流动注射分析串联质谱法取代检测甲卡西酮、氯胺酮和六种苯丙胺类兴奋剂的免疫分析法。

Replacing immunoassays for mephedrone, ketamines and six amphetamine-type stimulants with flow injection analysis tandem mass spectrometry.

机构信息

Department of Laboratory Medicine and Biotechnology, Tzu Chi University, Hualien, Taiwan.

出版信息

J Anal Toxicol. 2012 Oct;36(8):575-81. doi: 10.1093/jat/bks068. Epub 2012 Aug 29.

Abstract

A screening procedure was developed for the simultaneous detection of mephedrone, six amphetamine-type stimulants (ATS), ketamine and its two metabolites with electrospray ionization flow injection analysis tandem mass spectrometry (FIA-MS-MS). Urine samples were fortified with deuterated analogues as internal standards, extracted with ethyl acetate and analyzed with FIA-MS-MS. The mass analyzer was operated in multiple reaction monitoring mode. Two product ions were monitored for each drug and internal standards. For each analyte, the limit of detection was less than 4 µg/L, within-day and between-day precisions (percent coefficient of variation) at three different concentrations were less than 7.3% and bias was between -17.3 and 11.8%. Total analysis time with FIA-MS-MS is 1.8 min per sample. A group of 215 urine samples were screened with immunoassay for ATS and analyzed with FIA-MS-MS and gas chromatography-mass spectrometry (GC-MS) for ketamines and ATS. The analysis of ATS by immunoassay and GC-MS was 96.7% concordant. The analysis of three ketamines and seven ATS by FIA-MS-MS and GC-MS was 97.2% concordant. The FIA-MS-MS procedure is efficient, accurate, flexible and capable of detecting analytes of different chemical groups. It can replace immunoassays for the screening of new designer drugs when commercial immunoassays are unavailable.

摘要

建立了一种同时检测甲卡西酮、六种苯丙胺类兴奋剂(ATS)、氯胺酮及其两种代谢物的电喷雾电离流动注射分析串联质谱(FIA-MS-MS)筛选程序。尿样用氘代类似物作为内标进行强化,用乙酸乙酯提取,并采用 FIA-MS-MS 进行分析。质谱仪以多反应监测模式运行。每种药物和内标物均监测两个产物离子。对于每种分析物,检测限均小于 4μg/L,三个不同浓度下的日内和日间精密度(变异系数%)均小于 7.3%,偏差在-17.3%至 11.8%之间。每个样品的总分析时间为 FIA-MS-MS 1.8 分钟。用免疫分析法对 215 份尿液样本进行 ATS 筛查,并用 FIA-MS-MS 和气相色谱-质谱法(GC-MS)对氯胺酮和 ATS 进行分析。免疫分析和 GC-MS 对 ATS 的分析一致性为 96.7%。FIA-MS-MS 和 GC-MS 对三种氯胺酮和七种 ATS 的分析一致性为 97.2%。FIA-MS-MS 程序高效、准确、灵活,能够检测不同化学基团的分析物。当商业免疫分析法不可用时,它可以替代免疫分析法用于新的设计药物的筛选。

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