饲料中炔雌醚的液相色谱—串联质谱检测方法研究

摘要

This study established a HPLC-MS/MS method for the determination of quinestrol in feeds.Feed samples were firstly extracted by acetonitrile,then purified with C18 SPE column.The treated samples were analyzed by HPLC-MS/MS.The analysis was performed with multi reaction monitor(MRM) in positive ion mode.The results indicated good linearity with the concentration ranged from 1 to 400 μg/L for quinestrol.The limit of detection(LOD) and limit of quantitation (LOQ) were 0.01 and 0.05 mg/kg,respectively.While the spiked contents of quinestrol standard from 0.05 to 20 mg/kg,the recoveries and relative standard deviations(RSD) were in range of 67.3％～86.8％ and 1.30％～8.04％,respectively.The method was proved to be simple,rapid and reproducible for determination of quinestrol in feed.%本研究旨在建立饲料中炔雌醚含量测定的液相色谱-串联质谱检测方法.饲料样品用乙腈提取,C18SPE小柱净化,应用液相色谱-串联质谱仪,选择多反应监测(MRM)、正离子模式进行定性和定量分析.结果表明:炔雌醚在1～400 μg/L范围内线性关系良好,检出限为0.01 mg/kg,定量限为0.05 mg/kg;炔雌醚浓度在0.05～20 mg/kg的回收率为67.3％～86.8％,变异系数为1.30％～8.04％.本方法样品前处理简便、可靠,适用于各种饲料中炔雌醚的检测.