UPLC-MS/MS检测鸡蛋中胆酸及其衍生物  

Determination of cholic acid and derivative residues in eggs by UPLC-MS/MS

作　　者：周艳华[1] 李涛 徐文泱 汪霞丽 向俊 杨俊伟 ZHOU Yanhua;TI Tao;XU Wenyang;WANG Xiali;XIANG Jun;YANG Junwei(Changsha Environmental Protection College,Changsha,Hunan 410004,China;Hunan Institute of Commodity Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha,Hunan 410111,China)

机构地区：[1]长沙环境保护职业技术学院,湖南长沙410004 [2]湖南省产商品质量检验研究院食品安全监测与预警湖南省重点实验室,湖南长沙410111

出　　处：《食品与机械》2023年第12期38-41,64,共5页Food and Machinery

基　　金：湖南省自然科学基金项目(编号:2022JJ60098,2022JJ90027)。

摘　　要：目的:建立式固相萃取结合超高效液相色谱—串联质谱法(UPLC-MS/MS)检测鸡蛋中胆酸、去氧胆酸和去氢胆酸的方法。方法:样品经甲醇提取,PRiME HLB净化后,经C18色谱柱(100 mm×2.1 mm, 3.0μm)分离,甲醇—0.1%氨水溶液(体积分数)为流动相,梯度洗脱,负离子扫描和选择反应监测模式(SRM)检测,外标法定量。结果:胆酸(CA)、去氧胆酸(DCA)、去氢胆酸(DHCA)在0.5~500.0 ng/mL质量浓度范围内呈良好的线性关系,相关系数>0.999。CA、DCA和DHCA的检出限为1.0μg/kg,定量限为3.3μg/kg。在加标水平为1~10μg/kg, CA、DCA和DHCA加标回收率为93.7%~102.5%,RSD为1.8%~9.2%。对随机抽取的30批次鸡蛋进行检测,28批次样品检出胆酸。结论:该方法快速,灵敏度和准确度高,可作为鸡蛋中胆酸类药物及其衍生物的检测方法。Objective:The pretreatment method of through-type solid-phase extraction was improved to be coupled with ultra performance liquid chromatography tandem mass spectrometry for detection of cholic acid,deoxycholic acid and dehydrochloric in eggs.Methods:The samples were extracted by methanol and purified by PRiME HLB,then separated on C 18(100 mm×2.1 mm,3.0μm)column with methanol-0.1%ammonia as the mobile phase for gradient elution.Meanwhile,the samples were quantified by external standard with negative ion select reaction monitoring(SRM)mode.Results:The results showed that the linear relationships of cholic acid(CA),deoxycholic acid(DCA)and dehydrochloric acid(DHCA)were good in the range from 0.5 ng/mL to 500 ng/mL(R 2>0.999).The detection limits and quantitative limits of CA,DCA and DHCA were 1.0μg/kg and 3.3μg/kg.The average recovery of CA,DCA and DHCA from 1.0~10μg/kg were 93.7%~102.5%,with the RSD of 1.8%~9.2%.30 batches of randomly selected eggs were tested,and cholic acid was detected in all 28 batches of samples.Conclusion:This method is rapid with high sensitivity,accuracy,and it can be used as a method for the determination of cholic acid and derivative residues in eggs.

关 键 词：胆酸 去氧胆酸 去氢胆酸 鸡蛋 超高效液相色谱—串联质谱 

分 类 号：TS253.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]