气相色谱-串联质谱法测定牛奶中20种有机氯农药残留

Determination of 20 Organochlorine Pesticides Residues in Milk by Gas Chromatography-Tandem Mass Spectrometry

建立了牛奶中20种有机氯农药残留的气相色谱-串联质谱检测方法。样品采用正己烷-丙酮混合溶剂提取,凝胶渗透色谱和弗罗里硅土固相萃取联合净化,气相色谱-串联质谱测定。标准溶液在4μg/L-400μg/L范围内线性关系良好;方法的定量限为0.8μg/kg。20种有机氯农药在3个水平(0.8、2.0、10.0μg/kg)的加标回收率为62.2%-103.8%,相对标准偏差(RSDs)为3.4%-13.1%。该分析方法稳定可靠,灵敏度高,适合牛奶中多种有机氯农药残留量的检测。

A gas chromatography-tandem mass spectrometry（GC-MS /MS） method was developed for the determination of 20 organochlorine pesticides residues in milk.The samples were extracted by mixed solvent of n-hexene and acetone,purified by gel permeation chromatography and magnesiumtrisilicate solid phase extraction column,then detected by GC-MS/MS.The calibration curves showed good linearity in the range of 4μg/L-400μg /L.The limits of detection were 0.8μg/kg.The recoveries of 20 organochlorine pesticides in milk at the three spiked levels of 0.8,2,10μg/kg were in the range of 62.2%-103.8% with the relative standard deviations（RSDs） of 3.4%-13.1%.The method is stable and reliable,high sensitivity.