摘要
目的建立固相萃取-超高效液相色谱-串联三重四级杆质谱测定动物性食品中20种β-阻断剂兽药残留的检测技术。方法动物性食品样品经酸解提取后,经混合型阳离子交换柱净化,浓缩复溶后采用Waters ACQUITYTM BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,电喷雾正离子源和多反应监测扫描模式下进行测定,基质标准曲线结合稳定同位素内标法定量。结果20种β-阻断剂兽药阴性加标水平在1、2和4μg/kg下,回收率为61.9%~119.1%,相对标准偏差为1.5%~28.4%(n=6)。20种β-阻断剂兽药的检出限在0.01~0.15μg/kg,定量限在0.03~0.50μg/kg。对30件动物性食品样品进行了目标化合物的检测,未检测到相关β-阻断剂兽药残留。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,可为动物性食品中该类兽药残留的日常监控提供更方便、快捷的检测方法支持。
OBJECTIVE To establish an analytical method for determination of 20 kinds ofβ-receptor blockers residues in animal foods by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).METHODS The samples of animal foods were enzymatic hydrolysis by trichloroacetic acid(TCA),purified by MCX column.The separation was performed on a Waters ACQUITYTM BEH C18 column(100 mm×2.1 mm,1.7μm),then the target compounds were detected by UPLC-MS/MS with ESI positive ion scan in mode of multiple reaction monitoring(MRM)and quantified by matrix matched external standard method.RESULTS At the spiked level of 1,2 and 4μg/kg,the recoveries of each compound were in the range of 61.9%-119.1%with the relative standard deviations of 1.5%-28.4%(n=6).The qualitative limits of detections were 0.01-0.15μg/kg and the quantitative limits were 0.03-0.50μg/kg for the 20 targets compounds.By using the established method,the target compounds in 30 animal foods were detected,and no excessive veterinary drug residue were detected.CONCLUSION The established method is simple,rapid,high sensitivity and good stability,with a wide variety and a certain development.It can provide more convenient and fast detection method support for the daily monitoring of veterinary drug residues in animal foods.
作者
范赛
张楠
刘平
李丽萍
吴国华
赵榕
Fan Sai;Zhang Nan;Liu Ping;Li Liping;Wu Guohua;Zhao Rong(Beijing Center for Disease Prevention and Control,Beijing Research Center for Preventive Medicine,Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing 100013,China)
出处
《卫生研究》
CAS
CSCD
北大核心
2020年第5期829-835,867,共8页
Journal of Hygiene Research
