液相色谱-串联质谱法检测水产品中脱氢胆酸残留  

Determination of dehydrocholic acid residue in aquatic products by liquid chromatography-tandem mass spectrometry

作　　者：徐文泱 李灿 陈同强 向俊 XU Wenyang;LI Can;CHEN Tongqiang;XIANG Jun Hunan(Institute of Food Quality Supervision Inspection and Research,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410017)

机构地区：[1]湖南省食品质量监督检验研究院,食品安全监测与预警湖南省重点实验室,长沙410017

出　　处：《分析试验室》2022年第2期197-200,共4页Chinese Journal of Analysis Laboratory

基　　金：湖南创新型省份建设专项社会发展领域重点研发项目(2019SK2121);湖南省科技创新平台与人才计划项目(2019TP1058)资助。

摘　　要：采用液液萃取和SPE净化提取水产品中的脱氢胆酸,并建立液相色谱-串联质谱的检验方法。样品以乙酸乙酯和二氯甲烷提取后采用C_(18)柱进行分离,乙腈以及超纯水为流动相洗脱,电喷雾电离负离子模式扫描,多反应监测测定,外标法定量分析。标准溶液在0.05~2 ng/mL范围内呈线性关系,相关系数大于0.99,方法定量限为0.05μg/kg,平均回收率在90.4%~110.0%,相对标准偏差在6.5%~12%。Liquid-liquid extraction and solid phase extraction purification were used to extract dehydrocholic acid from aquatic products,and a liquid chromatography-tandem mass spectrometry method was established.The samples were extracted with ethyl acetate and dichloromethane,and then separated on C_(18) column with acetonitrile and ultrapure water as mobile phase.An electrospray ionization of negative ion mode scanning and multi-reaction monitoring were adopted for determination,and external standard calibration was used for quantitative analysis.The standard solution showed a linear relationship in the range of 0.05-2 ng/mL,the correlation coefficient was greater than 0.99,and the method quantification limit was 0.05μg/kg,with the average recovery of 90.4%-110.0%and the relative standard deviation of 6.5%-12%.

关 键 词：脱氢胆酸 水产品 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]