食品科学 ›› 2018, Vol. 39 ›› Issue (6): 307-314.doi: 10.7506/spkx1002-6630-201806048

• 安全检测 • 上一篇    下一篇

QuEChERS-气相色谱-串联质谱法测定蔬菜中35 种多氯联苯

谢思思,卢俊文,李蓉*,张宪臣,张朋杰,容裕棠,陈丽斯,谢丽芳   

  1. (中山出入境检验检疫局检验检疫技术中心,广东?中山 528400)
  • 出版日期:2018-03-25 发布日期:2018-03-14
  • 基金资助:
    广东省省级科技计划项目(2014A040401011;2015A050502010);广东检验检疫局科技计划项目(2017GDK24);中山市科技计划项目(2016B2168);中山市重大社会公益项目(2017B1029)

Determination of 35 Polychlorinated Biphenyls in Vegetables by Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) Extraction Coupled with Gas Chromatography-Tandem Mass Spectrometry

XIE Sisi, LU Junwen, LI Rong*, ZHANG Xianchen, ZHANG Pengjie, RONG Yutang, CHEN Lisi, XIE Lifang   

  1. (Inspection and Quarantine Technology Center, Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China)
  • Online:2018-03-25 Published:2018-03-14

摘要: 建立气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)法测定蔬菜中35 种多氯联苯的方法。样品用萃取柱、QuEChERS提取包两种方法进行提取比较其预处理效果,经无水硫酸镁脱水、乙二胺-N-丙基硅烷和石墨化炭黑净化,用GC-MS/MS在选择反应监测模式下进行测定,内标法定量。结果表明,35?种目标物在10~1?000?μg/L范围内呈良好线性,线性相关系数均大于0.999。方法检出限范围为0.65~18.12?ng/kg。在0.01、0.02、0.10?mg/kg?3?个加标水平下的平均回收率为72.3%~119.0%,相对标准偏差为0.4%~9.8%。该方法简单、快速、灵敏、准确,适用于蔬菜中多种多氯联苯残留量的快速测定。

关键词: QuEChERS, 气相色谱-串联质谱, 多氯联苯, 蔬菜

Abstract: A quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the determination of 35 polychlorinated biphenyls (PCBs) in vegetables. The sample was extracted using a solid-phase extraction column and QuEChERS with ethyl acetate as the extraction solvent, and then the extract was dried with anhydrous magnesium sulfate and cleaned up with primary secondary amine (PSA)/graphitized carbon black solid-phase extraction cartridge before being analyzed by GC-MS/MS under the selective reaction monitoring (SRM) mode and quantified by internal standard method. The results showed that the calibration curves for all target analytes displayed good linear relationships over the concentration range of 10-1 000 μg/L, with correlations coefficients of more than 0.999. The limits of detection (LODs) were 0.65-18.12 ng/kg. The average recoveries of 35 compounds at three spiked levels of 0.01, 0.02 and 0.10 mg/kg ranged from 72.3% to 119.0%, with relative standard deviations of 0.4% to 9.8%. The simplicity, rapidity, sensitivity and accuracy of the method make it suitable for rapid detection of PCB residues in vegetables.

Key words: QuEChERS, gas chromatography-tandem mass spectrometry (GC-MS/MS), PCBs, vegetables

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