高效液相色谱-串联质谱/质谱同时测定乳制品中4种β-受体激动剂残留量  

Determination of Clenbuterol,Salbutamol,Ractopamine and Terbutaline Residues in Dairy Products by High-Performance Liquid Chromatography-Tandem Mass Spectrometric/Mass Spectrometry Method

作　　者：吴云钊[1] 张晨[1] 孙潇 乔庆东[1] 曹民[1] 庄景新[1] WU Yunzhao;ZHANG Chen;SUN Xiao;QIAO Qingdong;CAO Min;ZHUANG Jingxin(Centers for Disease Prevention and Control of Changping,Bingjing 102200,China)

机构地区：[1]北京市昌平区疾病预防控制中心,北京102200

出　　处：《食品科技》2022年第8期294-301,共8页Food Science and Technology

摘　　要：目的:建立高效液相色谱-串联质谱/质谱同时测定乳制品中克伦特罗、沙丁胺醇、莱克多巴胺和特布他林4种β-受体激动剂残留量的方法。方法:样品以5%的三氯乙酸为水解提取液和蛋白沉淀剂,水浴超声提取后高速离心。提取液经正己烷除脂,过ProElut PCX固相萃取柱净化,除去干扰物。洗脱液经水浴氮吹至近干,用纯甲醇溶解后再次水浴氮吹至近干,流动相涡旋溶解,过0.22μm滤膜,高效液相色谱-串联质谱/质谱仪测定,采用正离子多反应监测(MRM)模式,内标法定量。结果:在优化后的色谱和质谱条件下,4种β-受体激动剂在浓度0.25~50.0 ng/mL,线性关系良好,线性相关系数(r)≥0.9951,方法检出限≤0.06μg/kg,不同基质中加标回收率为83.8%~118.7%,相对标准偏差(RSD)为4.2%~11.7%。结论:该方法样品前处理操作简单省时、净化效果好、分析效率和准确度高,可广泛适用于乳制品中克伦特罗、沙丁胺醇、莱克多巴胺和特布他林4种β-受体激动剂残留量的同时测定。Objective:To establish a high-performance liquid chromatography-tandem mass spectrometric/mass spectrometry(HPLC-MS/MS)method for the simultaneous determination of 4β-agonists in dairy products.clenbuterol,salbutamol,ractopamine and terbutaline.Methods:The sample was hydrolyzed and protein precipitated with 5% trichloroacetic acid as the extraction solution.After ultrasonic extraction in water bath,it was centrifuged at high speed.The extract is degreased by n-hexane and purified by solid phase extraction column(ProElut PCX)to remove interferents.The eluent is blown to near dry by nitrogen under water bath,dissolved with pure methanol,and then blown to near dry by nitrogen under water bath again.Mobile phase vortex dissolution,over 0.22μm filter membrane,determined by HPLC-MS/MS,using positive ion multi reaction monitoring(MRM)mode and quantitative by internal standard method.Results:Under the conditions of optimized chromatography and mass spectrometric,The calibration curves for the 4β-agonist residues were linear in the range of 0.25~50 ng/mL with the correlation coefficient of(r)≥0.9951,and the detection limits were less than 0.06μg/kg.The recovery rates of 4β-agonists residues from different matrices were 83.8%~118.7%,with relative standard deviation(RSD)range of 4.2%~11.7%.Conclusion:The method has the advantages of simple and time-saving sample pretreatment,good purification effect,high analysis efficiency and accuracy.It can be widely applied to clenbuterol,salbutamol,ractopamine and terbutaline in dairy products 4β-agonist residues simultaneous determination.

关 键 词：高效液相色谱-串联质谱 β-受体激动剂 固相萃取柱 乳制品 酸水解法 

分 类 号：TS207.53[轻工技术与工程—食品科学]