QuEChERS-液相色谱-串联质谱法测定3种β-受体激动剂

Determination of three kinds β-Agonists by QuEChERS-HPLC-MS/MS

通过QuEChERS前处理,液相色谱-串联质谱法测定克林特罗、莱克多巴胺、沙丁胺醇3种瘦肉精的残留量。样品用酸化乙腈提取,EMR-Lipid增强型脂质去除净化管和EMR-Lipid Polish反萃管净化,与水(2∶8,V/V)混合后过滤。采用ZORBAX C18(3.0 mm×150 mm,1.8μm)色谱柱为固定相,A 0.2%甲酸水(含2 mmol·L^(-1)乙酸铵)和B 0.2%甲酸甲醇作为流动相进行梯度洗脱,质谱采用电喷雾正离子模式(ESI+),动态多反应监测模式(MRM)进行测定。结果表明,此方法相关系数(r^(2))在0.999以上;在添加浓度为1.00μg·kg^(-1)、10.0μg·kg^(-1)、20.0μg·kg^(-1)时,回收率在100.2%~110.4%;相对标准偏差(RSD)在0.7%~3.1%(n=10)。该方法简化了净化流程,操作简便,准确度和精密度均满足食品检测要求,适用于畜肉中克林特罗、莱克多巴胺、沙丁胺醇残留量的测定。

Through QuEChERS pretreatment and liquid chromatography-tandem mass spectrometry,the residual amounts of clinbuterol,ractopamine,and salbutamol were determined.The sample was extracted with acidified acetonitrile,purified by EMR-Lipid enhanced lipid removal purification tube and EMR-Lipid Polish reverse extraction tube,mixed with water(2:8,V/V)and filtered.A ZORBAX C18(3.0 mm×150 mm,1.8μm)chromatographic column was used as the stationary phase,A 0.2% formic acid water(containing 2 mmol·L^(-1) ammonium acetate)and B 0.2% formic acid methanol were used as mobile phases for gradient elution.The electrospray positive ion mode(ESI+)and dynamic multiple reaction monitoring mode(MRM)were used for the determination.The results show that the correlation coefficient(r^(2))of this method is above 0.999;when the additive concentration is 1.00μg·kg^(-1),10.0μg·kg^(-1),20.0μg·kg^(-1),the recovery rate is 100.2%~110.4%;relative standard The deviation(RSD)is between 0.7%~3.1%(n=10).The method simplifies the purification process,is easy to operate,and has accuracy and precision that meet the requirements of food testing.It is suitable for the determination of clinbuterol,ractopamine,and salbutamol residues in livestock meat.