牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk

建立了同时快速检测牛奶中14种除草剂残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品采用乙腈提取,无水硫酸镁和无水乙酸钠净化,过0.22μm有机相滤膜后,目标物采用气相色谱-串联质谱(EI离子源)、多反应监测模式(MRM)检测。结果表明:在0.005~1 mg/L范围内,14种目标除草剂的质量浓度与其相应峰面积间呈良好的线性关系,决定系数(R^(2))均大于0.9902。在0.01、0.05和0.5 mg/kg 3个添加水平下,14种除草剂的平均回收率为76%~113%,相对标准偏差(RSD)为1.2%~8.6%(n=6)。14种除草剂在牛奶中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、操作步骤简单,适用于同时快速测定牛奶中14种除草剂的残留量。

A gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the simultaneous and rapid determination of 14 herbicides in milk was established.The samples were extracted with acetonitrile,cleaned-up with MgSO_(4)and Na_(2)AC,filtered through 0.22μm organic filter membrane,and the anlytes were determinated with GC-MS/MS(EI source and MRM mode).The results showed that the calibration curve was linear in the range of 0.005-1 mg/L and determination coefficient(R^(2))was higher than 0.9902.The average recoveries of 14 herbicides were 76%-113%and the relative standard deviations(RSD)were 1.2%-8.6%(n=6)when the spiked levels were 0.01,0.05 and 0.5 mg/kg.The limits of quantitation(LOQ)for 14 herbicides were 0.01 mg/kg.The method is accurate,sensitive,simple,and suitable for the simultaneous and rapid determination of 14 herbicides residues in milk.