超高效液相色谱-三重四极杆质谱法测定保健食品中30种非法添加壮阳类化合物  

Determination of 30 Anti-impotence Compounds Illegally Adulterated in Health Products by Ultrahigh Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：孙健[1] 胡青[1] 张甦[1] 冯睿[1] 于泓[1] 张静娴[1] 诸艳蓉[1] 毛秀红[1] 季申[1] SUN Jian;HU Qing;ZHANG Su;FENG Rui;YU Hong;ZHANG Jing-xian;ZHU Yan-rong;MAO Xiu-hong;JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《分析测试学报》2018年第4期419-426,共8页Journal of Instrumental Analysis

基　　金：2017年国家食品药品监督管理总局食品补充检验方法项目(食品中那非类物质的筛查);上海市科委技术平台专项(14DZ2294000);2017年上海市食品药品监督管理局课题(ZX-201710170017)

摘　　要：建立了超高效液相色谱-三重四极杆质谱测定保健食品中30种壮阳类化合物的方法。采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7μm),以0.1%(体积分数)甲酸水溶液-含0.1%(体积分数)甲酸的乙腈溶液为流动相,梯度洗脱,在电喷雾离子化正离子模式下,以多反应监测模式(MRM)检测。30种化合物在10~200μg/L范围内均呈良好的线性关系,相关系数均大于0.99;在0.1、0.2、1.0 mg/kg加标水平下的平均加标回收率为62.8%~135.2%,相对标准偏差均不大于14%(n=6);检出限为0.05 mg/kg,定量下限为0.1 mg/kg。该方法定性定量准确,操作简便,可为国家标准的建立提供参考。An analytical method was developed for the determination of 30 anti-impotence compounds illegally adulterated in health products by ultra high performance liquid chromatography-triple quadrupole mass spectrometry （UHPLC-MS/MS ） with a Waters CORTECS T3 （100 mm×2.1 mm,2.7 μm ） column using 0.1 % （by volume ） fomic acid aqueous solution-acetonitrile containing 0.1 % （by volume ） formic acid as mobile phases by gradient elution.The compounds were detected with electrospray ion source in positive mode under multiple reaction monitoring （MRM ） mode.The calibration curves for 30 targeted compounds were linear in the mass concentration range of 10-200 μg/L with correlation coefficients more than 0.99.The mean recoveries at spiked levels of 0.1,0.2,1.0 mg/kg were in the range of 62.8 % -135.2 % ,with RSDs （ n =6 ） not more than 14 % .The limits of detection （LODs ） and the limits of quantitation （LOQs ） were 0.05 mg/kg and 0.1 mg/kg,respectively.The established method is accurate and simple,and could be used as a reference for the national standard.

关 键 词：超高效液相色谱-三重四极杆质谱 非法添加 壮阳类化合物 保健食品 

分 类 号：O657.7[理学—分析化学] O657.63[理学—化学]