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在线免疫亲和色谱-高效液相色谱-质谱联用技术测定尿液中的药物

Determination of drugs from urine by on-line immunoaffinity chromatography-high-performance liquid chromatography-mass spectrometry.

作者信息

Rule G S, Henion J D

机构信息

Cornell University, Ithaca, NY 14850.

出版信息

J Chromatogr. 1992 Nov 6;582(1-2):103-12. doi: 10.1016/0378-4347(92)80308-d.

DOI:10.1016/0378-4347(92)80308-d
PMID:1491028
Abstract

A method for rapid extraction and identification of drugs in urine is described. The system utilizes a high-performance protein G immunoaffinity column coupled to a reversed-phase analytical column by use of a trapping column and switching valve. A small amount of antibody (5 micrograms drug-specific) is used for each analysis to extract either propranolol or lysergic acid diethylamide (LSD) from human urine. Urine diluted with phosphate-buffered saline is pumped directly through the protein G column thus eliminating time- and solvent-consuming sample preparation procedures. On-line ultraviolet or mass spectral analysis provides the means of drug detection and identification. With ultraviolet detection propranolol may be detected in spiked urine at the 250 pg/ml level. A Hewlett-Packard mass spectrometer modified for atmospheric pressure ionization and equipped with an ion spray source allows detection of propranolol in urine at 2.5 ng/ml and LSD at 500 pg/ml using single ion monitoring. The potential applicability of the technique for drug confirmations is discussed.

摘要

本文描述了一种尿液中药物的快速提取和鉴定方法。该系统利用高性能蛋白G免疫亲和柱,通过捕集柱和切换阀与反相分析柱相连。每次分析使用少量抗体(5微克药物特异性)从人尿中提取普萘洛尔或麦角酸二乙酰胺(LSD)。用磷酸盐缓冲盐水稀释的尿液直接泵入蛋白G柱,从而省去了耗时且费溶剂的样品制备程序。在线紫外或质谱分析提供了药物检测和鉴定的手段。采用紫外检测时,加标尿液中普萘洛尔的检测限为250 pg/ml。一台经过大气压电离改装并配备离子喷雾源的惠普质谱仪,使用单离子监测可检测尿液中2.5 ng/ml的普萘洛尔和500 pg/ml的LSD。讨论了该技术在药物确证方面的潜在适用性。

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