气相色谱-质谱联用技术用于利尿剂的快速初筛和确证  

Rapid Screening and Confirmation of Diuretics with Macroprogram by Gas Chromatography-Mass Spectrometry

作　　者：刘薇[1] 邱丽君[1] 上官良敏[1] 张兰[1] 

机构地区：[1]福州大学食品安全分析与检测教育部重点实验室,运动科学研究中心,福州350002

出　　处：《分析化学》2008年第11期1465-1470,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20675016);福建省体育局重大专项(No.HX2005-74);福建省自然科学基金(No.2007J0279);福建省教育厅科技计划项目(No.2007F5067);福建世纪优秀人才支持计划(No.HX2006-101);福州大学科技发展基金(No.2006-XY-07)资助项目

摘　　要：利用微波辅助衍生及宏程序技术,对反兴奋剂条例的禁用列表中的一系列利尿剂药物进行了研究。建立了同时分析尿样中9种利尿剂的气相色谱-质谱联用（GC/MS）测定以及抽检尿样的初筛、确证的新方法。在GC-MS的选择离子监测（SIM）模式下,所建立定量方法的检出限为0.3-6.6μg/L;尿样中的提取回收率为37.6%-96.8%;RSD小于9.7%。由于采用了微波衍生样品前处理技术和宏程序数据处理方法,显著提高了分析效率,不但检测灵敏度完全能满足国际奥委会的要求,而且检测时间缩短3 h以上。方法成功地应用于口服吲达帕胺后尿样的检测,探讨了人尿中吲达帕胺代谢情况,有效进行兴奋剂监控提供了依据。A monitoring process using macroprogram（ in SIM mode） to accelerate screening analysis of diuretics in human urine with subsequent confirmation by SCAN mode was established for improving their analysis efficiency. Microwave assisted derivatization was adopted for acceletating pretreatment speed. Nine kinds of diuretics in human urine were quantitativly detected by GC-MS with selected ion monitoring technique. The detection limit of these diuretics was 0.3 - 6.6 μg/L, the average recovery was 37.6% - 96.8% and the RSD 〈9.7%. Using of advanced microwave assisted derivatization pretreatment technique and macroprogram data processing method, the analysis time decreased for 3 h and sensitivity completely satisfied for WADA. This method was also successfully applied to identify the indapamide positive urine, and the excretion curve of indapamide in human urine was described.

关 键 词：气相色谱-质谱 利尿剂 宏程序 微波辅助衍生 

分 类 号：R87[医药卫生—运动医学]