摘要
建立超高效液相色谱—串联质谱法同时检测保健食品中5种降脂类药物(洛伐他汀、辛伐他汀、美伐他汀、去羟基洛伐他汀、洛伐他汀羟酸钠盐)的方法,样品以甲醇超声提取后,用Waters Acquity HSS T3色谱柱分离,乙腈—0.1%甲酸水溶液梯度洗脱,流速为0.3mL/min,电喷雾离子源正负离子同时扫描,多反应监测(MRM)方式检测,外标法定量。结果表明:该条件下5min内可准确地定性定量分析5种化合物,分离度好,检出限为15μg/kg,定量限为50μg/kg,加标回收率为94.6%～105.7%。用此方法检测17批市售降血脂保健食品,其中1批次样品测出洛伐他汀、洛伐他汀羟酸钠盐、去羟基洛伐他汀。该方法简便、快速、灵敏、准确,适合于保健食品中的洛伐他汀及其类似物的快速测定。
A ultra-high performance liquid chromatographytandem mass spectrometric(UPLC-MS/MS)assay method has been developed and fully validated for the simultaneous quantification of lovastatin,simvastatin,mevastatin,lovastatin sodium hydroxide,dehydro lovastatin.The samples were extracted with methanol and separated on a Waters Acquity HSS T3 column.The mobile phase consisting of 0.1%aqueous formic acid solution and acetonitrile using gradient elution at a flow rate of0.3 mL/min.The positive and negative ions were scanned simultaneously.The multiple reaction monitoring(MRM)mode was used for detection.The results showed that the five compounds were separated well within five minutes.The limits of detection and the limits of quantification were 15μg/kg and 50μg/kg,respectively.The recoveries were between 94.6%~105.7%,and the relative standard deviation of the methods were lower than10%.17 batches of hypolipidemic health food were tested by this method,lovastatin,lovastatin sodium hydroxide salt and dehydro lovastatin were detected in one batch of samples.The method was simple,rapid,sensitive and accurate,and it was suitable for the rapid determination of lovastatin and its analogues in functional foods.
作者
韩智
龚蕾
王会霞
朱晓玲
王彬
曹琦
吴婉琴
HAN Zhi;GONG Lei;WANG Hui-xia;ZHU Xiao-ling;WANG Bin;CAO Qi;WU Wati-qin(Hubei Provincial Institute for Food Supervision and Test,Wuhan,Hubei 430070,China;Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test,Wuhan,Hubei 430070,China)
出处
《食品与机械》
北大核心
2019年第3期58-62,共5页
Food and Machinery
基金
国家重点研发计划资助(编号:2018YFC1604000)
关键词
超高效液相色谱串联质谱
保健食品
洛伐他汀类似物
ultra-high performance liquid chromatography-tandem mass spectrometric ( UPLC-MS/MS)
functional foods
lovastatin and its analogues
作者简介
韩智,男,湖北省食品质量安全监督检验研究院助理工程师,硕士;通信作者:王会霞(1973—),女,湖北省食品质量安全监督检验研究院高级工程师,硕士。E-mail:972567848@qq.com.
