基于硅胶整体柱的压力辅助毛细管电色谱-电喷雾电离质谱联用技术用于快速分析麻醉药品。

Pressure-assisted capillary electrochromatography with electrospray ionization-mass spectrometry based on silica-based monolithic column for rapid analysis of narcotics.

作者信息

Lu Minghua, Zhang Lan, Feng Qiang, Xia Shifei, Chi Yuwu, Tong Ping, Chen Guonan

机构信息

Ministry of Education Key Laboratory of Analysis and Detection Technology for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian, P. R. China.

出版信息

Electrophoresis. 2008 Feb;29(4):936-43. doi: 10.1002/elps.200700653.

DOI:10.1002/elps.200700653

PMID:18213603

Abstract

A pressure-assisted CEC (pCEC) with ESI-MS based on silica-based monolithic column was developed for rapid analysis of narcotics. Combining the extremely high permeability and separation efficiency of silica-based monolithic column with the high selectivity and sensitivity of pCEC-ESI-MS, the developed system exhibited its prominent advantages in separation and detection. A systematic investigation of the pCEC separation and ESI-MS detection parameters was performed. Experiment results showed that the optimized separation efficiency could be obtained at 8 bar assisted pressure with 25 kV separation voltage, using the solution containing 65% ACN v/v and 20 mmol/L ammonium acetate with pH 6.0 as running buffer. 3 microL/min of sheath liquid was considered as the optimized flow rate since it could provide the maximum signal intensity. Under the optimum conditions, the tested five narcotics could be completely separated within 10 min with the detection limit in the range of 2.0-80 nmol/L. The proposed method has been successfully used for detection of narcotics in real urine samples.

摘要

基于硅胶整体柱开发了一种结合电喷雾电离质谱（ESI-MS）的压力辅助毛细管电色谱（pCEC）方法，用于快速分析麻醉药品。该系统将硅胶整体柱的极高渗透率和分离效率与pCEC-ESI-MS的高选择性和灵敏度相结合，在分离和检测方面展现出显著优势。对pCEC分离和ESI-MS检测参数进行了系统研究。实验结果表明，以含65%（体积分数）乙腈、20 mmol/L醋酸铵且pH值为6.0的溶液作为运行缓冲液，在8 bar辅助压力和25 kV分离电压下可获得优化的分离效率。3 μL/min的鞘液流速被视为优化流速，因为它能提供最大信号强度。在最佳条件下，5种被测麻醉药品能在10 min内完全分离，检测限在2.0 - 80 nmol/L范围内。该方法已成功用于实际尿液样本中麻醉药品的检测。