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基于微流控芯片的纳升级液相色谱-串联质谱法测定人发中滥用药物及其代谢物。

Microfluidic chip based nano liquid chromatography coupled to tandem mass spectrometry for the determination of abused drugs and metabolites in human hair.

机构信息

Division of Life Science, The Hong Kong University of Science and Technology, Hong Kong.

出版信息

Anal Bioanal Chem. 2012 Mar;402(9):2805-15. doi: 10.1007/s00216-012-5711-6. Epub 2012 Jan 27.

Abstract

A microfluidic chip based nano-HPLC coupled to tandem mass spectrometry (nano-HPLC-Chip-MS/MS) has been developed for simultaneous measurement of abused drugs and metabolites: cocaine, benzoylecgonine, cocaethylene, norcocaine, morphine, codeine, 6-acetylmorphine, phencyclidine, amphetamine, methamphetamine, MDMA, MDA, MDEA, and methadone in the hair of drug abusers. The microfluidic chip was fabricated by laminating polyimide films and it integrated an enrichment column, an analytical column and a nanospray tip. Drugs were extracted from hairs by sonication, and the chromatographic separation was achieved in 15 min. The drug identification and quantification criteria were fulfilled by the triple quardropule tandem mass spectrometry. The linear regression analysis was calibrated by deuterated internal standards with all of the R(2) at least over 0.993. The limit of detection (LOD) and the limit of quantification (LOQ) were from 0.1 to 0.75 and 0.2 to 1.25 pg/mg, respectively. The validation parameters including selectivity, accuracy, precision, stability, and matrix effect were also evaluated here. In conclusion, the developed sample preparation method coupled with the nano-HPLC-Chip-MS/MS method was able to reveal the presence of drugs in hairs from the drug abusers, with the enhanced sensitivity, compared with the conventional HPLC-MS/MS.

摘要

基于微流控芯片的纳升级高效液相色谱-串联质谱(nano-HPLC-Chip-MS/MS)已被开发出来,用于同时检测滥用药物及其代谢物:可卡因、苯甲酰古柯碱、古柯卡因、去甲可卡因、吗啡、可待因、6-乙酰吗啡、苯环利定、苯丙胺、甲基苯丙胺、摇头丸、MDA、MDEA 和海洛因。微流控芯片通过层压聚酰亚胺薄膜制成,集成了一个富集柱、一个分析柱和一个纳米喷雾尖端。通过超声处理从头发中提取药物,在 15 分钟内实现了色谱分离。三重四极杆串联质谱法满足了药物鉴定和定量标准。所有的 R(2) 至少都在 0.993 以上,通过氘代内标进行线性回归分析。检测限(LOD)和定量限(LOQ)分别为 0.1 至 0.75 和 0.2 至 1.25 pg/mg。还评估了验证参数,包括选择性、准确性、精密度、稳定性和基质效应。总之,与传统的 HPLC-MS/MS 相比,开发的样品制备方法与 nano-HPLC-Chip-MS/MS 方法相结合,能够更灵敏地揭示滥用药物者头发中的药物存在情况。

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