QuEChERS-气相色谱-串联质谱测定牛奶中有机氯农药及多氯联苯的分析

建立快速测定牛奶中有机氯及多氯联苯残留量的气相色谱-串联质谱（gas chromatography-tandem mass spectrometry，GC-MS/MS）分析方法。样品经30%硫酸-甲醇预处理，正己烷提取，QuEChERS净化，GC-MS/MS测定，基质标准曲线定量。结果表明，待测物质在5～200?μg/L范围内线性关系良好，相关系数大于0.99，检出限为0.1～0.3?μg/kg，样品平均加标回收率为85.5%～115.2%，相对标准偏差小于10%（n=6）。该方法简单、准确、高效，可用于牛奶样品中有机氯及多氯联苯残留的快速筛查和定量检测。

Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Milk by QuEChERS-Gas Chromatography-Tandem Mass Spectrometry

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the analysis of organochlorine pesticides (OCP) and polychlorinated biphenyls (PCBs) in milk. Samples were?pre-processed with 30% sulfuric acid-methanol, and then extracted with n-hexane. The supernatant extract was puri?ed by a modi?ed quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction procedure, and the?purified extract was detected by GC-MS/MS and quantified by the matrix standard calibration curve method. The results showed that all the target analytes displayed good linear relationships in the range of 5–200 μg/L with correlation coefficients more than 0.99. The limits of detection (LODs) of OCPs and PCBs ranged from 0.1 to 0.3 μg/kg. The average recoveries of OCPs and PCBs from spiked samples were in the ranges of 85.5%–115.2%, with relative standard deviations (RSDs) less than 10% (n = 6). In summary, the proposed method due to its simplicity, high accuracy and ef?ciency could be used for the rapid screening and quantitative analysis of organochlorine pesticide and polychlorinated biphenyls in milk.