固相微萃取技术用于牛奶中有机氯类农药残留的检测

建立了固相微萃取(SPME)-气相色谱-串联质谱(GC-MS/MS)同时测定牛奶中16种有机氯类农药残留的方法。对萃取模式、纤维涂层、萃取温度等实验条件进行了优化。用HP-5 MS弹性石英毛细管柱经柱程序升温技术分离,并用质谱检测器检测,外标法计算含量。待测农药的标准加入回收率在80%～110%之间,方法的相对标准偏差(RSD)≤9.6%,各农药组分的检出限为0.003μg/kg～0.15μg/kg。所测样品不含几种有机氯农药残留。本法简便、干扰小、检测效果好,可用于牛奶中有机氯类农药残留的检测。

Determination of Organochlorine Pesticide Residues in Milk by SPME

A method was developed for determination of 16 organochlorine pesticides （OCPs） in milk by solid-phase microextraction （SPME） and gas chromatography-tandem mass spectrometry （GC-MS/MS） detection. SPME conditions, including SPME extraction mode, fibre types, extraction temperature have been evaluated and optimized. The pesticides were finally separated and detected by GC-MS/MS with multiple reaction monitoring （MRM） mode. The recoveries for 16 OCPs standards spiked samples were between 80% and 110%. The precisions of developed method with relative standard deviation were lower than 9.6%. Limits of detection （3σ ） was 0.003μg/kg -0.15 μg/kg. The OCPs were not detected in all the samples we analyzed. The method is easy to operation, and with good precision, it is therefore well suited for the analysis of OCPs in milk.