摘要
建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测14种药食同源动物性食品中4种甾体激素的方法。样品采用TLC分离法,以乙腈为提取溶剂,以硅胶为分离介质,三氯甲烷-乙醚-甲醇-浓氨水(40︰3︰4︰1,V/V)为展开剂,在254 nm紫外光灯下检视定位,进行前处理,采用Kinetex 100 RP-18色谱柱分离,以乙腈-5 mmol/L乙酸铵(含0.1%甲酸)溶液为流动相梯度洗脱,采用电喷雾-正负离子同时监测的多反应监测模式,基质匹配外标法定量,检测诺龙、己烯雌酚、氢化可的松和醋酸氯地孕酮等4种药物。结果显示,4种甾体激素线性范围在0.5~500μg/L,线性关系良好,各组分的检出限在0.13~0.27μg/kg,定量限在0.46~0.61μg/kg。不同样品中的待测物分别在3个加标水平(0.5,1.0和2.0μg/kg)下的平均回收率为68.2%~100.1%,变异系数≤16.1%(n=5)。该方法可用于14种药食同源动物性食品中的4种甾体激素的快速筛查和定量测定。
A method for simultaneous determination of 4 drugs added in animal foods for both medicine and food was established by thin-layer chromatography and ultra performance liquid chromatography tandem mass spectrometry(UPLCMS/MS).The samples were extracted by TLC,and were subsequently separated on a Kinetex 100 RP-18 column with the gradient elution.The mobile phase consisted of 5 mmol/L of ammonium acetate solution(with 0.1%formic)and acetonitrile.MRM mode was used to quantify the 4 drugs with the name nandrolone,stilbestrol,hydrocortisone and chlormadinone acetate.The results showed that the 4 drugs had good linear relationships in the range of 0.5-500μg/L;LOD was 0.13-0.27μg/kg,and LOQ was 0.46-0.61μg/kg.The average recoveries(0.5,1.0 and 2.0μg/kg)were in the range of 68.2%to 100.1%,and the relative standard deviations(n=5)were less than 16.1%.The established method was suitable for rapid screening and quantification of the 4 added drugs in the animal supplies for both medicine and food.
作者
曹晓琴
方振峰
张涛
施璐
CAO Xiaoqin;FANG Zhenfeng;ZHANG Tao;SHI Lu(College of Medicine,Jianghan University,Wuhan 430056)
出处
《食品工业》
CAS
2021年第5期422-426,共5页
The Food Industry
基金
江汉大学高层次人才科研启动项目(08250001)。
关键词
薄层层析
超高效液相色谱-串联质谱
药食同源动物性食品
残留检测
thin-layerchromatography(TLC)
ultra performance liquid chromatography-tandem mass spectrometry(UPLCMS/MS)
animal foods for both medicine and food
residue detection
