高效液相色谱-串联质谱法同时测定鸡肉、鸡蛋中喹乙醇和卡巴氧及代谢物残留  

Simultaneous determination of residues of carbadox, olaquindox and related metabolites in chicken and egg by high performance liquid chromatography-tandem mass spectrometry

作　　者：张静[1] 高玉时[1] 唐梦君[1] 万玉 马丽娜[1] 周倩[1] 张小燕[1] 杨星星 赵敏 ZHANG Jing;GAO Yu-Shi;TANG Meng-Jun;WAN Yu;MA Li-Na;ZHOU Qian;ZHANG Xiao-Yan;YANG Xing-Xing;ZHAO Min(Jiangsu Institute of Poultry Science,Yangzhou 225125,China)

机构地区：[1]江苏省家禽科学研究所,扬州225125

出　　处：《食品安全质量检测学报》2019年第2期469-475,共7页Journal of Food Safety and Quality

基　　金：扬州市社会发展面上项目(YZ2017079);国家自然科学青年基金项目(31700005);2018国家畜禽产品风险评估专项(GIFP201800702)~~

摘　　要：目的建立高效液相色谱-电喷雾电离串联质谱法测定鸡肉、鸡蛋中喹乙醇、卡巴氧及其代谢物残留量的分析方法。方法组织样品中的卡巴氧和喹乙醇用乙腈-乙酸乙酯(1:1, V:V)溶液提取;代谢物的提取用蛋白酶酶解后经盐酸溶液酸化,采用阴离子交换固相萃取柱净化和富集。分析样品以0.1%甲酸溶液-甲醇进行梯度洗脱,经Waters Xbridge C_(18)色谱柱分离,以液相色谱串联质谱多反应监测(multiple reaction monitoring,MRM)正离子模式进行检测。结果 5种喹喔啉类药物在0.5～50ng/mL浓度范围内线性良好,相关系数r^2为0.9956～0.9988;该方法的检出限和定量限分别为0.1～0.5μg/kg和1.0～2.0μg/kg;鸡蛋和鸡肉样品中,喹乙醇、卡巴氧、脱氧卡巴氧、喹喔啉-2-羧酸和3-甲基喹喔啉-2-羧酸在0.2～2.0μg/kg加标水平的平均回收率为85.1%～108.2%,日内精密度为4.9%～8.7%,日间精密度为6.2%～11.7%。结论该方法简单有效、回收率好、灵敏度高、特异性好,能满足日常检测的需求。Objective To establish a method for the simultaneous identification and determination of residues of carbadox,olaquindox and related metabolites in chicken and egg by high performance liquid chromatography-tandem mass spectrometry with electrospray ionization.Methods Carboxyl and olaquindox from tissue samples were extracted with acetonitrile-ethyl acetate(1:1,V:V) solution.The metabolites were acidized by hydrochloric acid after protease enzymolysis,and then cleaned up with anion solid-phase extraction cartridge.The separation of compounds were carried on a Waters Xbridge C18 column by gradient elution using acetonitrile-0.1% formic acid as mobile phase,and analyzed by high performance liquid chromatography-tandem mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode(MRM).Results The 5 quinolines had good linear relationships in the range of 0.5-50 ng/mL,and the correlation coefficients were 0.9956-0.9988.The limits of detection and the limits of quantification were 0.1-0.5 μg/kg and 1.0-2.0 μg/kg,respectively.The average recoveries of olaquindox,carbadox,desoxycarbadox,quinoxalie-2-carboxylic acid,and methyl-3-quinoxaline-2-carboxylic acid in egg and chicken samples of 0.2-2.0 μg/kg were 85.1%-108.2%,and intra-day precision and inter-day precision were 4.9%-8.7% and 6.2%-11.7%,respectively.Conclusion This method is simple and effective,with good recovery,high sensitivity and specificity,which can meet the needs of daily detection.

关 键 词：卡巴氧 喹乙醇 脱氧卡巴氧 喹喔啉-2-羧酸 3-甲基喹喔啉-2-羧酸 鸡肉 鸡蛋 高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]