食品科学 ›› 2018, Vol. 39 ›› Issue (8): 309-313.doi: 10.7506/spkx1002-6630-201808048

• 安全检测 • 上一篇    下一篇

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

付文雯,罗彤,朱影,周陶鸿,文红,王会霞*   

  1. (湖北省食品质量安全监督检验研究院,湖北?武汉 430000)
  • 出版日期:2018-04-25 发布日期:2018-04-17

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

FU Wenwen, LUO Tong, ZHU Ying, ZHOU Taohong, WEN Hong, WANG Huixia*   

  1. (Hubei Provincial Institute for Food Supervision and Test, Wuhan 430000, China)
  • Online:2018-04-25 Published:2018-04-17

摘要: 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。

关键词: 气相色谱-串联质谱(GC-MS/MS), QuEChERS, 有机氯农药, 多氯联苯, 牛奶

Abstract: 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.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), QuEChERS, organochlorine pesticides, polychlorinated biphenyls, milk

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