超高效液相色谱-三重四级杆质谱法测定牛干巴中2种喹噁啉类药物残留  

Determination of 2 kinds of quinoxaline drug residues in dry-cured beef by ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry

作　　者：马晓年[1] 陈俊秀 张瑞雨[1] 欧利华[1] 张秀清 MA Xiao-Nian;CHEN Jun-Xiu;ZHANG Rui-Yu;OU Li-Hua;ZHANG Xiu-Qing(Kunming Center for Disease Control and Prevention, Kunming 650228, China)

机构地区：[1]云南省昆明市疾病预防控制中心

出　　处：《食品安全质量检测学报》2019年第11期3362-3366,共5页Journal of Food Safety and Quality

基　　金：昆明市卫生人才科技人才培养项目(2017-sw(后备)-66)~~

摘　　要：目的建立超高效液相色谱-三重四级杆质谱法测定牛干巴中卡巴氧及喹赛多的含量的分析方法。方法样品经乙酸乙酯-乙腈提取,正己烷脱色净化后,以乙腈-0.1%甲酸溶液为流动相,经ACQUITYTMBEH18柱分离,采用多反应监测正离子模式进行定性及定量分析。结果卡巴氧及喹赛多的检出限分别为0.2和2.0μg/kg,3个加标水平回收率范围为66.4%~115.0%,相对标准偏差为4.2%~8.2%。结论该方法灵敏度高、重复性好、准确度高、分析时间短、样品前处理操作简便,适用于牛干巴中卡巴氧及喹赛多的测定。Objective To establish a method for the determination of carbadox and cyadox in dry-cured beef by ultra performance liquid chromatography/triple qudrupole tandem mass spectrometry. Methods The dry-cured beef sample was extracted with ethyl acetate-acetonitrile, and then decolorizated and purificated with N-hexane. Target compounds were separated with ACQUITYTMBEH18 column with acetonitrile-water (0.1% formate) as mobile phase, and then characterized by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode (MRM). Results Limits of detection of carbadox and cyadox were 0.2 μg/kg and 2.0 μg/kg, respectively. The recoveries at 3 spiked concentrations were from 66.4% to 115.0% and the relative standard deviations were from 4.2%-8.2%. Conclusion This method has higher sensitivity, good repeatability, higher accuracy, shorter analysis time and convenient sample pretreatment, which is suitable for the detection of carbadox and cyadox in dry-cured beef.

关 键 词：卡巴氧 喹赛多 牛干巴 超高效液相色谱-三重四级杆质谱法 

分 类 号：O657.63[理学—分析化学]