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通过式固相萃取柱结合QuEChERS前处理技术-液相色谱串联质谱法快速测定熟肉食品中4种β2-受体激动剂残留

Rapid determination of 4 kinds of β2-agonist residues in cooked meat by pass-through solid phase extraction column combined with QuEChERS pretreatment technique-liquid chromatography tandem mass spectrometry

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【作者】 王莉莉; 张楠; 刘平; 刘伟; 李丽萍; 吴国华; 赵榕; 范赛;

【Author】 WANG Li-Li;ZHANG Nan;LIU Ping;LIU Wei;LI Li-Ping;WU Guo-Hua;ZHAO Rong;FAN Sai;Beijing Center for Disease Prevention and Control, Beijing Center for Prevention Medicine Research, Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning;

【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;

【摘要】 目的建立通过式固相萃取柱结合前处理技术-液相色谱串联质谱法快速测定熟肉制品中克伦特罗、莱克多巴胺、沙丁胺醇、特布他林4种常见β2-受体激动剂类兽药残留的分析方法。方法熟肉制品采用5%三氯乙酸酸解, NaCl盐析乙腈萃取,正己烷除脂后经通过式固相萃取柱和QuEChERS净化,超高效液相色谱-串联质谱于电喷雾正离子源(ESI+)和多反应监测扫描模式下进行测定,基质匹配标准曲线外标法定量。结果 4种目标化合物阴性加标水平在2、5、10mg/kg下,回收率在77.2%~104.7%之间,相对标准偏差在2.9%~9.6%之间。4种目标化合物的检出限在0.2~0.6mg/kg之间,定量限在0.6~2.0mg/kg之间。对30件熟肉样品进行目标化合物的检测,未检测到β2-受体激动剂类兽药残留。结论该方法操作简便、快速,灵敏度和准确度高,包含种类较宽,具有一定的拓展性,适用熟肉制品相关残留的日常监测。

【Abstract】 Objective To establish a method for the rapid determination of veterinary drug residues of 4 common β2-receptor agonists in cooked meat products, including clenbuterol, ractopamine, salbutamol, and terbutaline, by pass-through solid-phase extraction column combined with pretreatment technique-liquid chromatography tandem mass spectrometry. Methods The cooked meat products were subjected to acidolysis with 5% trichloroacetic acid, extraction with NaCl salting-out acetonitrile, and degreased with n-hexane, which were then purified by passing through a solid-phase extraction column and QuEChERS. The ultra-performance liquid chromatography-tandem mass spectrometry was performed in electrospray positive ion source(ESI+) and multi-reaction monitoring scanning mode. The matrix matching standard curve was quantified by external standard method. Results The recoveries of the 4 target compounds were 77.2%-104.7% and the relative standard deviation was 2.9%-9.6% at the negative spiked levels of 2, 5, and 10 mg/kg, respectively. The detection limits of the 4 target compounds were 0.2-0.6 mg/kg, and the quantitative limits were 0.6-2.0 mg/kg. Thirty cooked meat samples were tested for the target compound and no residue of β2-receptor agonist veterinary drug was detected. Conclusion This method is simple, rapid, sensitive and accurate, has a wide range of types, and has certain expansibility. It is suitable for the daily monitoring of related residues of cooked meat products.

  • 【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09期
  • 【分类号】O657.63;TS251.7
  • 【被引频次】2
  • 【下载频次】153
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