高效液相色谱-串联质谱法同时测定血清中游离和结合型胆汁酸  

Simultaneous Determination of Free and Conjugated Bile Acids in Serum by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：丁敏[1] 叶炼[1] 王猛[1] 邵勇[2] 

机构地区：[1]重庆医科大学医学检验系临床检验诊断学省部共建教育部重点实验室,重庆400016 [2]重庆医科大学附属第一医院妇产科,重庆400016

出　　处：《分析化学》2007年第10期1506-1508,共3页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.20475069)

摘　　要：建立了高效液相色谱-串联质谱同时测定血清中游离和结合型胆汁酸的方法。血清样品经固相萃取后，在C18色谱柱上梯度洗脱，用负离子多反应监测模式检测。15种胆汁酸在0．10～100．0μmol／L的浓度范围内与响应呈良好的线性，r为0．9990～0．9999；检出限为0．001～0．006μmol／L；本方法的相对标准偏差日内不超过3．0％，日间不超过6．0％；平均回收率为86．0％～110．0％，适合于临床检测血清胆汁酸。A method has been developed for the determination of individual free and conjugated bile acids by liquid chromatography tendem mass spectrometry （HPLC-MS/MS）. Bile acids were extracted from serum samples using cartridges and eluted using gradient on a C18 column. Electrospray ionisation （ESI） was performed in the negative ion mode. The elutions were monitored in multiple reaction-monitoring mode. The linear ranges of the method were 0. 10 - 100.0 μmol/L with the correlation coeffients from 0.9990 to 0.9999 for all bile acids. The detection limit ranged from 0.001 to 0.006 μmol/L. The intra-day precisions were below 3.0% and the inter-day precisions were below 6.0% for all bile. The average recoveries of the extraction procedure were between 86.0% and 110.0%. The developed method was suitable for the routine clinical practice.

关 键 词：胆汁酸 血清 高效液相色谱 串联质谱 

分 类 号：R446.1[医药卫生—诊断学]