牛肉和牛肝中4种β-受体激动剂类药物残留量的全自动固相萃取-同位素内标-超高压液相色谱串联质谱测定法  

Determination of four kinds of β-agonists in beef and bovine liver with automated solid phase extraction-isotope internal standards by ultra-high-pressure liquid chromatography-tandem triple quadrupole mass spectrometry

作　　者：江恩源[1] 朱国强[1] 劳哲[1] 喻梁洪 JIANG En-yuan;ZHU Guo-qiang;LAO Zhe;YU Liang-hong(Physical&Chemical Inspection Section,W uzhou Municeipal Center Jfor Disease Control and Prerention,Wuzhou Guangri,543002 China)

机构地区：[1]梧州市疾病预防控制中心理化检验科,广西梧州543002

出　　处：《职业与健康》2022年第13期1761-1764,共4页Occupation and Health

摘　　要：目的 建立一种全自动固相萃取-同位素内标-超高压液相色谱串联质谱法测定牛肉和牛肝中4种β-受体激动剂残留的方法。方法 样品用乙酸钠-乙酸缓冲液(0.2 mol/L,pH=5.2)提取,离心后经全自动SLS固相萃取(solid phase extraction,SPE)柱净化,用Shim-pack GISS C18色谱柱(50 mm×2.1 mm,1.9μm)进行色谱分离,以电喷雾正离子多反应监测模式进行测定,内标法定量。结果 4种β-受体激动剂的标准曲线的线性范围均是0.3~10.0μg/kg,相关系数均r>0.999 7,相关性良好,最低检出限(the limits of detection,LOD)均为0.1μg/kg,最低定量限(the limits of quantification,LOQ)均为0.3μg/kg。加标平均回收率为90.1%~94.5%,相对标准偏差(the relative standard deviation,RSD)为3.9%~6.0%。结论 该方法操作便捷,准确度和灵敏度较高,精密度较好,适用于牛肉和牛肝中4种β-受体激动剂残留的测定。Objective To develop a method for determination of four kinds of β-agonists in beef and bovine liver with automated solid phase extraction-isotope internal standards by ultra-high-pressure liquid chromatography-tandem triple quadrupole mass spectrometry. Methods The sample was extracted by sodium acetate-acetic acid buffer(0.2 mol/L,pH=5.2),and purified through automated solid phase extraction(SPE) column after centrifugation. The extract components were separated on the Shim-pack GISS C18 column(50 mm×2.1 mm,1.9 μm),and detected under electrospray positive ion multiple reaction monitoring(MRM) mode. It was analyzed with internal standard method for quantification. Results The linear ranges of standard curve for four kinds ofβ-agonists were 0.3-10.0 μg/kg,the correlation coefficients(r) were 0.999 7,showing good correlation. The limits of detection(LOD) were all 0.1 μg/kg and the limits of quantification(LOQ) were all 0.3 μg/kg. The average recovery rate of standard addition was 90.1%-94.5%,and the relative standard deviation(RSD) was 3.9%-6.0%. Conclusion The method is easy to operate,with high accuracy,sensitivity and precision,which is suitable for the determination of four kinds of β-agonists residuals in beef and bovine liver.

关 键 词：质谱 同位素内标 β-受体激动剂 全自动固相萃取 

分 类 号：R115[医药卫生—公共卫生与预防医学]