碱水解-SPE-HPLC-MS/MS法检测乳制品中喹乙醇及代谢物

Determination of Olaquindox and Its Metabolites in Dairy Products by Alkali Hydrolysis-SPE-HPLC-MS/MS

建立一种快速、高效的SPE-HPLC-MS/MS测定乳制品中的喹乙醇及代谢物的方法。样品前处理采用碱水解提取喹乙醇和MQCA,经MAX小柱净化后检测。以乙腈-0.1%氨水为流动相,在质谱检测器的多反应监测模式下进行分析。结果表明,喹乙醇和MQCA在0.1~50.0 ng/mL质量浓度范围内线性良好,相关系数R2为0.9992~0.9997,检出限均为5.0μg/kg,定量限均为20μg/kg。加标试验分别添加40,100和200μg/kg 3个浓度,加标回收率达到81.6%~97.1%(n=5)。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,适用于乳制品中的喹乙醇及代谢物残留量的检测和确证。

To establish a rapid and efficient SPE-HPLC-MS/MS method for the determination of olaquindox and its metabolites in dairy products.The sample was pretreated by alkali hydrolysis to extract olaquindox and MQCA,and then purified by MAX column.Using acetonitrile-0.1%ammonia as mobile phase,the analysis was carried out under the multi reaction monitoring mode of mass spectrometer.The results showed that the linearity of olaquindox and MQCA was good in the concentration range of 0.1~50.0 ng/mL the correlation coefficient R2 was 0.9992~0.9997,the detection limit was 5.0μg/kg,and the quantitative limit was 20μg/kg.Three concentrations of 40,100 and 200μg/kg were added in the standard addition experiment,and the recovery rate was 81.6%~97.1%(n=5).This method has the advantages of simple pretreatment,good purification effect,high sensitivity and fast detection speed.It is suitable for the detection and confirmation of olaquindox and its metabolites in dairy products.