超高效液相色谱-串联质谱法检测卤肉中4种β-受体激动剂残留
Determination of 4 Kinds of β-Agonists Residues in Braised Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
孟春杨 1吴玉田 1彭蕾 1钟雪 1邹璐 1刘文政 1周贻兵1
作者信息
- 1. 贵州省疾病预防控制中心,贵州贵阳 550004
- 折叠
摘要
建立了一种超高效液相色谱串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS)检测卤肉中 4种β-受体激动剂(特布他林、克仑特罗、莱克多巴胺、沙丁胺醇)的方法.样品经β-盐酸葡萄糖醛酸苷酶/芳基硫酸酯酶解后,经SLS固相萃取柱净化.以 0.1%甲酸水和乙腈为流动相梯度洗脱,用Thermo Hypersil Gold C18 色谱柱分离,ESI+进行多反应监测(MRM),内标法定量.4种β-受体激动剂在浓度为 0.5～9.5 μg/L范围内线性关系良好,相关系数(r)均大于 0.9988,检出限(LOD)为 0.1 μg/kg,定量限(LOQ)为 0.3 μg/kg.3个加标水平下(1、5、9 μg/kg)的回收率在 87.9%～113.7%之间,RSD为 1.48%～9.32%.162批次卤肉样品,有一份卤猪蹄样品检出克伦特罗含量为 1.51 μg/kg,莱克多巴胺为 3.65 μg/kg;另外一份卤羊肉样品检出克伦特罗含量 11.5 μg/kg.本方法快速准确,可用于卤肉中 4种β-受体激动剂(特布他林、克仑特罗、莱克多巴胺、沙丁胺醇)的定性、定量检测.
Abstract
An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS)method was developed for the determination of four β-agonists(terbutaline,clenbuterol,ractopamine,salbutamol)in braised meat.Samples were hydrolyzed by β-glucuronidase and cleaned up by an SLS solid phase extraction column.The separation was performed on a Thermo Hypersil Gold C18 column with a gradient elution of 0.1%formic acid water and acetonitrile as mobile phases,ESI+ was used for multiple response monitoring(MRM)and quantitative analysis by internal standard method.The linear relationship of the four β-agonists was good in the concentration range of 0.5 μg/L to 9.5 μg/L,and the correlation coefficient(r)was greater than 0.9988.The limit of detection(LOD)was 0.1 μg/kg,and the limit of quantitation(LOQ)was 0.3 μg/kg.The recoveries were 87.9%～113.7%and RSDs were 1.48%～9.32%at three spiked levels(1,5 and 9 μg/kg).In a total of 162 batches of braised meat samples,one sample of braised pig's trotter was found to contain 1.51 μg/kg of clenbuterol and 3.65 μg/kg of ractopamine.Additionally,another sample of braised lamb was found to contain 11.5 μg/kg of clenbuterol.The method is rapid and accurate,and can be used for qualitative and quantitative determination of fourβ-agonists(terbutaline,clenbuterol,ractopamine,salbutamol)in braised meat.
关键词
超高效液相色谱串联质谱(UPLC-MS)/卤肉/β-受体激动剂/SLS固相萃取柱/同位素内标Key words
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS)/braised meat/β-agonists/SLS solid phase extraction column/isotope internal standard引用本文复制引用
基金项目
贵州省卫生健康委科学技术基金(gzwkj2022-268)
贵州省科学(青年)技术基金(2021-E1-2 青)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据