SPE-HPLC-MS/MS法检测动物源性运动食品中喹乙醇及卡巴氧代谢物残留

建立一种快速、高效的固相萃取-高效液相色谱-串联质谱法（SPE-HPLC-MS/MS）测定动物源性运动食品中的3-甲基-喹喔啉-2-羧酸（MQCA）及喹恶啉-2-羧酸（QCA）的方法。样品前处理采用碱水解提取MQCA和QCA，经PAX固相萃取柱（60 mg/3 mL）净化后检测。以乙腈-0.1%甲酸溶液为流动相，在质谱检测器的多反应监测（MRM）模式下进行分析。结果表明，MQCA和QCA在0.1～50.0 ng/mL质量浓度范围内线性关系良好，相关系数R2为0.999 6～0.999 8，检出限均为0.05 μg/kg，定量限均为0.20 μg/kg。平均加标回收率为83.67%～96.08%，精密度试验结果相对标准偏差（RSD）为1.75%～3.10%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于动物源性运动食品中的MQCA及QCA残留量的检测。

Determination of olaquindox and carbadox metabolites residues in animal derived sports food by SPE-HPLC-MS/MS

A rapid and efficient SPE-HPLC-MS/MS method for the determination of 3-methyl-quinoxaline-2-carboxy (MQCA) and quinoxaline-2-carboxylic acid (QCA) in animal derived sports food was established. The sample was pretreated by alkali hydrolysis to extract MQCA and QCA, and determined after purification by PAX solid phase extraction column (60 mg/3 ml). The acetonitrile-0.1% formic acid solution was used as mobile phase, and the analysis was carried out under multi reaction monitoring (MRM) mode of mass spectrometer. The results showed that the linearity of MQCA and QCA was good in the concentration range of 0.1-50.0 ng/ml, the correlation coefficient R2 was 0.999 6-0.999 8, the detection limit was 0.05 μg/kg, and the quantitative limit was 0.20 μg/kg. The average standard recovery rate was 83.67%-96.08%, and the relative standard deviation (RSD) of precision test results was 1.75%-3.10%. The method had the advantages of simple pretreatment, good purification effect, high sensitivity and fast detection speed, which was suitable for the detection of MQCA and QCA residues in animal derived sports food.