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液相微萃取结合高效液相色谱法测定人尿中的局部麻醉剂。

Liquid-phase microextraction combined with high-performance liquid chromatography for the determination of local anaesthetics in human urine.

作者信息

Ma Ming, Kang Shaoying, Zhao Qian, Chen Bo, Yao Shouzhuo

机构信息

State Key Laboratory of Chemo/Biosensing and Chemometrics, Hunan University, Changsha 410082, PR China.

出版信息

J Pharm Biomed Anal. 2006 Jan 23;40(1):128-35. doi: 10.1016/j.jpba.2005.06.023. Epub 2005 Aug 1.

Abstract

A simple liquid-phase microextraction (LPME) device combined with high-performance liquid chromatography (HPLC) is presented for the simultaneous analysis of local anaesthetics, lidocaine, bupivacaine, and tetracaine, from human urine sample. An organic solvent showed good compatibility with the mobile phase of the HPLC, o-dibutyl phthalate, was selected. Local anaesthetics are extracted from 6 ml of the feed aqueous solution and human urine sample into a water-immiscible organic solvent suspended at the needle tip of the microsyringe, then the organic solvent was directly introduced to a reversed-phase HPLC system. The kind of the organic extraction solvent, the stirring rate, the pH value of the aqueous feed solution, and the extraction time have been discussed. Under the optimized extraction conditions, high enrichment factors (more than 86.0-fold) and significant sample clean-up for all of studied local anaesthetics were achieved within 30 min. The detection limits (lower than 0.05 microg/ml) were comparable with previously reported gas chromatography methods. This method was applied to specimen of patient who was treated with extradural anaesthesia of lidocaine, bupivacaine, and tetracaine, and revealed that simultaneous determination of above three local anaesthetics in human urine was possible.

摘要

本文介绍了一种结合高效液相色谱(HPLC)的简单液相微萃取(LPME)装置,用于同时分析人尿液样本中的局麻药利多卡因、布比卡因和丁卡因。选择了一种与HPLC流动相具有良好兼容性的有机溶剂邻苯二甲酸二丁酯。将局麻药从6 ml的进料水溶液和人尿液样本中萃取到悬浮在微量注射器针尖处的与水不混溶的有机溶剂中,然后将有机溶剂直接引入反相HPLC系统。讨论了有机萃取溶剂的种类、搅拌速率、进料水溶液的pH值和萃取时间。在优化的萃取条件下,30分钟内所有研究的局麻药均实现了高富集因子(超过86.0倍)和显著的样品净化。检测限(低于0.05μg/ml)与先前报道的气相色谱法相当。该方法应用于接受利多卡因、布比卡因和丁卡因硬膜外麻醉治疗的患者样本,结果表明可以同时测定人尿液中的上述三种局麻药。

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