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β_(2)-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β_(2)-受体激动剂类兽药化合物空白样本加标水平在2.5、12.5、50μg/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0.1~0.3μg/kg,定量限为0.3~1.0μg/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β_(2)-受体激动剂类兽药残留快速检测。
Objective To a establish a method for the rapid determination of 4 β_(2)-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 β_(2)-agonist veterinary drug compounds in blank samples were spiked at 2.5,12.5,and 50μg/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 0.1‒0.3μg/kg,and the limits of quantification were 0.3‒1.0μg/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 β_(2)-agonist veterinary drug residues clenbuterol,ractopamine,salbutamol,and terbutaline in beef.
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
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,Beijing 100013,China;Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing 100013,China;China Shanghai Anpu Experimental Technology Co.,Ltd.,Shanghai 201609,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第11期4647-4653,共7页
Journal of Food Safety and Quality
关键词
β_2-受体激动剂类兽药
液相色谱-串联质谱法
CNW兽药定量检测分散固相萃取纯化包
β_(2)-agonist veterinary drugs
liquid chromatography tandem mass spectrometry
CNW veterinary drug quantitative detection and dispersive solid phase extraction purification method
