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基质分离固相萃取-液相色谱-串联质谱法快速测定牛肉中4种β2-受体激动剂类兽药残留

Rapid determination of 4 kinds of β2-agonist veterinary drug residues in beef by matrix separation solid phase extraction purification combined with liquid chromatography-tandem mass spectrometry

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【作者】 王莉莉; 陈雪营; 张楠; 刘平; 刘伟; 李丽萍; 吴国华; 赵榕; 范赛; 闫薪竹;

【Author】 WANG Li-Li;CHEN Xue-Ying;ZHANG Nan;LIU Ping;LIU Wei;LI Li-Ping;WU Guo-Hua;ZHAO Rong;FAN Sai;YAN Xin-Zhu;Beijing Center for Disease Prevention and Control,Beijing Center for Prevention Medicine Research;Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning;China Shanghai Anpu Experimental Technology Co.,Ltd.;

【通讯作者】 赵榕;范赛;

【机构】 北京市疾病预防控制中心北京市预防医学研究中心; 食物中毒诊断溯源技术北京市重点实验室; 上海安谱实验科技股份有限公司;

【摘要】 目的建立基质分离固相萃取结合液相色谱串联质谱法(liquidchromatographytandemmass spectrometry, LC-MS/MS)快速测定牛肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林等4种β2-受体激动剂类兽药残留。方法样品经葡萄糖醛苷酶/硫酸酯酶酶解、盐析后经CNW兽药定量检测分散固相萃取纯化包净化。采用LC-MS/MS电喷雾正离子模式、多反应监测采集(multiple reaction monitoring acquisition, MRM)测定。结果当4种β2-受体激动剂类兽药化合物空白样本加标水平在2.5、12.5、50mg/kg时,回收率为95.39%~106.59%,相对标准偏差(relative standard deviation, RSD)为0.98%~13.26%。4种目标化合物的检出限为0.1~0.3mg/kg,定量限为0.3~1.0mg/kg。针对市售66件牛肉样品中目标化合物进行检测,结果均未检出。结论与传统通过性固相萃取法相比,兽药定量检测分散固相萃取纯化法净化效果更好,基质效应更低。CNW兽药定量检测分散固相萃取法可用于牛肉中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林4种β2-受体激动剂类兽药残留快速检测。

【Abstract】 Objective To a establish a method for the rapid determination of 4 β2-agonist veterinary drug residues in beef, including clenbuterol, ractopamine, salbutamol and terbutaline by matrix separation solid phase extraction combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods The samples were hydrolyzed by gluconidase/sulfatase, salted out, purified by CNW veterinary drug quantitative detection and dispersive solid phase extraction purification method, and determined by LC-MS/MS electrospray positive ion mode and multiple reaction monitoring acquisition(MRM). Results When the standard levels of 4 kinds of β2-agonist veterinary drug compounds in blank samples were spiked at 2.5, 12.5, and 50 mg/kg, the recoveries were 95.39%-106.46%, and the relative standard deviation were 0.98%-13.26%. The limits of detection of the 4 kinds of target compounds were 0.1-0.3 mg/kg, and the limits of quantification were 0.3-1.0 mg/kg. The target compounds were detected in 66 beef samples on the market, but the results were not detected. Conclusion Compared with the traditional solid-phase extraction method, quantitative determination of veterinary drugs dispersive solid phase extraction purification method has better purification effect and lower matrix effect. CNW veterinary drug quantitative detection dispersive solid-phase extraction method can be used for rapid detection of 4 kinds of β2-agonist veterinary drug residues clenbuterol, ractopamine, salbutamol, and terbutaline in beef.

  • 【文献出处】 食品安全质量检测学报 ,Journal of Food Safety & Quality , 编辑部邮箱 ,2021年11期
  • 【分类号】O657.63;TS251.52
  • 【被引频次】1
  • 【下载频次】144
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