Captiva EMR-Lipid固相萃取结合UPLC-MS/MS测定炖肉中非法添加去痛片中4种成分  

Determination of 4 Chemicals in Qutong Tablets Illegally Added in Stew by Captiva EMR-Lipid Solid Phase Extraction with UPLC-MS/MS

作　　者：李志梅 刘萌 张亮 陈芳芳 张晶 隋玉杰 LI Zhimei;LIU Meng;ZHANG Liang;CHEN Fangfang;ZHANG Jing;SUI Yujie(Wenzhou Institute for Food and Drug Control,Wenzhou 325000,China)

机构地区：[1]温州市食品药品检验科学研究院,浙江温州325000

出　　处：《现代食品》2022年第12期184-188,共5页Modern Food

基　　金：浙江省市场监督管理局雏鹰计划核心项目(CY2022227);温州市基础性农业科技项目(N20210002)。

摘　　要：目的:建立采用Captiva EMR-Lipid前处理结合超高效液相色谱-串联质谱法测定炖肉中非法添加去痛片中4种成分(氨基比林、咖啡因、非那西丁与苯巴比妥)的外标方法。方法:样品经酸化乙腈提取,Captiva EMR-Lipid固相萃取柱净化,用0.05%甲酸(含5 mmol·L^(-1)乙酸胺)水溶液和乙腈作为流动相洗脱分离,采用电喷雾-正/负离子MRM模式检测。结果:在1~200 ng·mL^(-1)的质量浓度,4种化合物的线性相关系数均大于0.995,该方法的检出限在0.6~2.5μg·kg^(-1)。肉制品进行3个水平添加实验(n=6),4种化合物的回收率为85.1%~113.1%,RSD为0.81%~14.60%。结论:本方法快速准确、精密度高,适合于炖肉中非法添加去痛片中4种成分的检测。Objective:To establish an external standard for the determination of four components(aminopyrine,caffeine,phenacetin and phenobarbital)in stew illegally added to Qutong tablets using Captiva EMR-Lipid pretreatment combined with UPLC-MS/MS method.Method:The samples were extracted with acidified acetonitrile,purified by Captiva EMR-Lipid solid phase extraction column,eluted with 0.05%formic acid(containing 5 mmol·L^(-1) amine acetate)aqueous solution and acetonitrile as mobile phases,and separated by electrospray-positive/negative ion MRM mode detection.Result:In the mass concentration range of 1~200 ng·mL^(-1),the linear correlation coefficients of the four compounds were all greater than 0.995,and the detection limit of this method was 0.6~2.5μg·kg^(-1).Three levels of addition experiments were performed on meat products(n=6).The recoveries of the four compounds were 85.1%~113.1%,and the RSD were 0.81%~14.60%.Conclusion:The method is fast,accurate and high in precision,and is suitable for the detection of four components in the illegally added Qutong tablets in stew.

关 键 词：Captiva EMR-Lipid固相萃取 非法添加 去痛片 炖肉 

分 类 号：O657.63[理学—分析化学]