超高效液相色谱-串联质谱法测定鸡肉与鸡蛋中6种他汀类药物残留  

Determination of Statins Residues in Chicken and Egg by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：陈吉汉[1,2] 路勇[3] 姜洁[3] 冯楠[3] 傅泽田[1] 侯彩云[1] 

机构地区：[1]中国农业大学,北京100083 [2]中国农业大学食品科学与营养工程学院教育部-北京市共建功能乳品重点实验室,北京100083 [3]北京市食品安全监控中心,北京100041

出　　处：《分析化学》2014年第2期209-214,共6页Chinese Journal of Analytical Chemistry

基　　金：北京市科委计划基金(No.Z121100000312014)资助项目

摘　　要：建立了超高效液相色谱-串联质谱法（UPLC-MS/MS）测定鸡肉与鸡蛋中6种他汀类药物残留量的方法。采用BEH C18色谱柱,以甲醇-0.1%甲酸5 mmol乙酸铵为流动相,梯度洗脱分离,在电喷雾正负离子模式下以多反应监测（MRM）方式检测,外标法定量。6种他汀类药物检出限（LOD,S/N=3）和定量限（LOD,S/N=10）分别为0.1~0.5μg/kg和0.3~2.0μg/kg,在1.0~100μg/kg浓度范围内线性良好,相关系数大于0.9910;鸡肉和鸡蛋样品中20μg/kg水平的加标回收率分别为80.9%~97.2%和79.0%~87.2%,相对标准偏差分别为1.3%~10.2%和1.5%~10.7%。本方法应用于市场实际样品检测,尚未检出阳性样品。An analytical method based on ultra performance liquid chromatography tandem mass spectrometry has been developed for the simultaneous determination of 6 statins residues in Chicken and egg. The statins were analyzed on an ACQUITY UPLC BEH C18 column（ 100 mm ×2.1 mm,1.7μm） , using the methanol -5 mmol ammonium acetate （added 0.1% formic acid） as the mobile phase and a gradient elution program with a cycle time of 20 min, detected by electrospray ionization mass spectrometry in both positive and negative mode with multiple reaction monitoring, quantified by external standard method. The limits of detection （LOD, S/N=3） and quantification （LOQ, S/N= 10） of 6 statins were 0. 1-0. 5 p,g/kg and 0. 3- 2.0 μg/kg, respectively. The correlation coefficients of linear calibration curve were over 0. 9910 in the ranges of 1.0-100μg/kg. Average fortified recoveries in Chicken and egg samples were 80.9% -97.2% and 79.0%-87.2% at the spiked level of 20 μg/kg, and the relative standard deviations were 1.3%-10.2% and 1.5% -10.7% , respectively.

关 键 词：液相色谱-串联质谱 他汀类药物 药物残留 鸡肉 鸡蛋 

分 类 号：R155.5[医药卫生—营养与食品卫生学]