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

中文关键词:  β2-受体激动剂  熟肉制品  超高效液相色谱串联质谱法  QuEChERS  通过式固相萃取柱

英文关键词:β2-receptor agonists  cooked meat products  liquid chromatography tandem mass spectrometry  QuEChERS  pass-through solid phase extraction column

中文摘要:

      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、10 ?g/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0.2~0.6 ?g/kg之间, 定量限在0.6~2.0 ?g/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。

英文摘要:

      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 ?g/kg, respectively. The detection limits of the 4 target compounds were 0.2?0.6 ?g/kg, and the quantitative limits were 0.6?2.0 ?g/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.