超高效液相色谱-四极杆-飞行时间质谱对血清中结合型胆汁酸的定性分析研究  

Qualitative analysis of conjugated bile acids in human serum by ultra-performance liquid chromatography coupled with electrospray ionization-time of flight-mass spectrometry

作　　者：陈德莹[1] 苏小玲[1] 李君[1] 曹红翠[1] 李兰娟[1] 

机构地区：[1]浙江大学医学院附属第一医院传染病诊治国家重点实验室,杭州310003

出　　处：《药物分析杂志》2013年第8期1303-1310,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：浙江省自然科学基金资助项目(No.LY13D060004)

摘　　要：目的:采用超高效液相色谱-四极杆-飞行时间质谱仪,负离子模式下定性分析血清中结合型胆汁酸。方法:利用全信息串联质谱(MSE)技术,在1次液质分析中同时获得高精确离子质量的母离子及碎片离子信息,利用两者具有的相同色谱行为特性进行母-子离子的关联归属,定性分析血清中结合型胆汁酸。结果:分析健康人血清与肝病患者血清中结合型胆汁酸,最终定性出4种甘氨结合型胆汁酸(G-BAs),4种甘氨结合型胆汁酸硫酸酯(G-BA-Ss),4种牛磺结合型胆汁酸(T-BAs)和1种牛磺结合型胆汁酸硫酸酯(T-BA-S)。结论:建立全信息串联质谱技术(MSE)法鉴定血清中结合型胆汁酸,为胆汁异常相关疾病的研究提供了良好的分析工具。Objective： To analyze human serum by ultra-performance liquid chromatography-electrospray ionization-quadrupole-time of flight-mass spectrometry（UPLC-ESI-Q-TOF-MS）,in negative ionization mode.Methods： MSE data collection technique was used,where information of both parent ions and fragment ions of highly accurate ion mass was simultaneously acquired in one liquid-mass analytical run.The association of parent daughter ions was identified by their common characteristics of chromatographic behaviors,thus the conjugated bile acid in serum was further analyzed qualitatively.Results： Analysis of serum conjugated bile acid in patients and healthy individual was conducted based on the consistency of chromatographic behavior of the parent and fragment ions.As a result,4 G-BAs（glycine-bile acids）,4 G-BA-Ss（glycine-bile acids sulfates）,4 T-BAs（taurine-bile acids） and 1 T-BA-S（taurine-bile acid sulfate） had been unequivocally identified in the human plasma.Conclusion： A simple method based on MSE data collection mode to identify the conjugated bile acids in human serum is established,which provides a research tool for studying hepatobiliary diseases.

关 键 词：血清样品 生物样品 甘氨结合型胆汁酸 牛磺结合型胆汁酸 超高效液相色谱-飞行时间质谱 全信息串联质谱技术 

分 类 号：R917[医药卫生—药物分析学]