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

中文关键词:  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

英文关键词:carbadox  olaquindox  desoxycarbadox  quinoxalie-2-carboxylic acid  methyl-3-quinoxaline-2-carboxylic acid  chicken  egg  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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 C18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0.5~50 ng/mL浓度范围内线性良好, 相关系数r2为0.9956~0.9988; 该方法的检出限和定量限分别为0.1~0.5 μg/kg和1.0~2.0 μg/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0.2~2.0 μg/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。

英文摘要:

      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.