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 ofβ-agonist residues in cooked meat by pass-through solid phase extraction column combined with QuEChERS pretreatment technique-liquid chromatography tandem mass spectrometry

作　　者：王莉莉[1] 张楠[1] 刘平[1] 刘伟[1] 李丽萍[1] 吴国华[1] 赵榕[1] 范赛[1] 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,Beijing 100013,China)

机构地区：[1]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,北京100013

出　　处：《食品安全质量检测学报》2021年第9期3771-3776,共6页Journal of Food Safety and Quality

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。Objective To establish a method for the rapid determination of veterinary drug residues of 4 commonβ2-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 ofβ2-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.

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 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]