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牛羊毛发中3种β-受体激动剂药物残留测定的EMR-Lipid方法研究OACSTPCD

Method for determination of doping drug desidues with cattle and sheep hair as target tissues based on the EMR-Lipid technology

中文摘要英文摘要

旨在建立一种以牛羊毛发为靶标结合强化基质去除技术(EMR-Lipid)对 3 种β-受体激动剂药物(克伦特罗、莱克多巴胺、沙丁胺醇)残留量进行测定的方法.毛发样品经选取、清洗、干燥、研磨后,经酸水解和氨化乙腈提取后加入到Captiva EMR-Lipid净化柱,加入石墨化炭黑(GCB)进行净化,过滤后用高效液相色谱-串联质谱仪进行测定,采用正离子(ESI+)扫描,多反应监测(MRM)模式进行分析,内标法定量.结果显示:待测药物在0.1~100 ng/mL的浓度范围内具有良好的线性相关性,相关系数R2≥0.995;方法检测限(LOD)为 0.2 μg/kg,定量限(LOQ)为 0.5 μg/kg;药物在 1、20、100 μg/kg添加浓度下,平均回收率为 70%~120%,相对标准偏差≤20%.该方法取样方便,前处理步骤少,灵敏度和精密度高,符合残留检测要求,为动物性产品中β-受体激动剂类药物残留量测定提供了参考.

A UPLC-MS/MS method was developed using the enhanced matrix removal technology(EMR-Lipid)for rapid determination of residues of β-receptor agonist drugs(clenbuterol,ractopamine,salbutamol)in cattle and sheep hair.The samples to be tested were pre-pared by selecting,cleaning,drying and grinding.After acid hydrolysis and ammonified acetonitrile extraction,the hair samples were poured into the Captiva EMR-Lipid purification columns.The ultra-high performance liquid chromatography-tandem mass spectrometry instrument equipped with an ESI+electric spray ion source was used for determination under a multi-reaction monitoring mode(MRM),and the internal standard method was applied for quantitative analysis.The results showed that the linear range of the drug had a good linear correlation in the concentration range of 0.1-100 ng/mL,and the correlation coefficient was≥0.995.The limit of detection(LOD)of this method was 0.2 μg/kg,and its limit of quantification(LOQ)was 0.5 μg/kg.The average recovery rate of the drugs was 70%-120%,and its relative stand-ard deviation was≥20%at concentrations of 1,20,100 μg/kg of the drugs.To sum up,the present method was convenient for sampling,with less pre-treatment steps,high sensitivity and precision;which would meet the residue detection requirements and might serve as refer-ence for determination of residues of β-receptor agonists in animal products.

李文辉;孙志文;于寒冰;倪香艳;张晶晶;魏紫嫣;王乐宜;赵雅妮;赵莹;方芳

北京市农产品质量安全中心, 北京 102600

畜牧业

牛羊毛发β-受体激动剂EMR-Lipid技术残留检测

cattle and sheep hairβ-receptor agonistsEMR-Lipid technologyresidue detection

《畜牧与兽医》 2024 (002)

55-61 / 7

北京市农业科技项目(20170311);北京市农业农村局配套项目(202101)

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