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 ofβ-Agonists Residues in Braised Meat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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 C_(18)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0.5~9.5μg/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0.1μg/kg,定量限(LOQ)为0.3μg/kg。3个加标水平下(1、5、9μg/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1.51μg/kg,莱克多巴胺为3.65μg/kg;另外一份卤羊肉样品检出克伦特罗含量11.5μg/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。

An ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS)method was developed for the determination of fourβ-agonists(terbutaline,clenbuterol,ractopamine,salbutamol)in braised meat.Samples were hydrolyzed byβ-glucuronidase and cleaned up by an SLS solid phase extraction column.The separation was performed on a Thermo Hypersil Gold C_(18) 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 fourβ-agonists was good in the concentration range of 0.5μg/L to 9.5μg/L,and the correlation coefficient(r)was greater than 0.9988.The limit of detection(LOD)was 0.1μg/kg,and the limit of quantitation(LOQ)was 0.3μg/kg.The recoveries were 87.9%~113.7%and RSDs were 1.48%~9.32%at three spiked levels(1,5 and 9μg/kg).In a total of 162 batches of braised meat samples,one sample of braised pig’s trotter was found to contain 1.51μg/kg of clenbuterol and 3.65μg/kg of ractopamine.Additionally,another sample of braised lamb was found to contain 11.5μg/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.