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.
作者
孙健
胡青
张甦
冯睿
于泓
张静娴
诸艳蓉
毛秀红
季申
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
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)
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
ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS )
illegal adulteration
anti-impotence compounds
health products