食品科学 ›› 2020, Vol. 41 ›› Issue (4): 300-306.doi: 10.7506/spkx1002-6630-20181019-212

• 安全检测 • 上一篇    下一篇

气相色谱-串联质谱法高通量检测食用油中3 类污染物

孟维一,古瑾,姜锐,张晴,赵文涛,马燕红,赵奕昕,李莹莹,郭文萍   

  1. (1.中国肉类食品综合研究中心,北京 100068;2.北京工业大学生命科学与生物工程学院,北京?100020)
  • 出版日期:2020-02-25 发布日期:2020-03-02
  • 基金资助:
    北京市优秀人才培养资助项目(2016754154700G147); 国家重点研发计划“食品安全关键技术研发”重点专项(2017YFC1601706)

High-Throughput Detection of Three Types of Contaminants in Edible Oils by Gas Chromatography-Tandem Mass Spectrometry

MENG Weiyi, GU Jin, JIANG Rui, ZHANG Qing, ZHAO Wentao, MA Yanhong, ZHAO Yixin, LI Yingying, GUO Wenping   

  1. (1. China Meat Research Center, Beijing 100068, China;2. College of Life Science and Bio-engineering, Beijing University of Technology, Beijing 100020, China)
  • Online:2020-02-25 Published:2020-03-02

摘要: 建立气相色谱-三重四极杆串联质谱同时测定食用油中的18 种邻苯二甲酸酯、16 种多环芳烃和7 种多氯联苯的检测方法。样品经正己烷饱和乙腈超声提取、固相萃取柱净化,采用DB-5毛细管柱分离,以电子电离源,多反应离子监测模式定量测定。该方法邻苯二甲酸酯类塑化剂的线性范围为0.04~2 mg/kg,其中邻苯二甲酸二异壬酯的线性范围为1~40 mg/kg,多环芳烃和多氯联苯的线性范围为0.01~0.4 mg/kg,各物质在相应质量浓度范围内线性关系良好,相关系数均大于0.99。方法检出限范围为0.08~2 μg/kg(除邻苯二甲酸二异壬酯的检出限为8 μg/kg),回收率在62.7%~128.3%之间,相对标准偏差在1.1%~13.6%之间(n=6)。该方法准确、灵敏、简单、快速,可用于食用油中18 种邻苯二甲酸酯、16 种多环芳烃和7 种多氯联苯的定量测定。

关键词: 气相色谱-三重四极杆串联质谱, 邻苯二甲酸酯, 多环芳烃, 多氯联苯, 食用油

Abstract: In this paper, a gas chromatography-tandem mass spectrometry (GC-MS) method was established for the determination of 18 phthalates, 16 polycyclic aromatic hydrocarbons and 7 polychlorinated biphenyls in edible oils. The sample was ultrasonically extracted with acetonitrile saturated by n-hexane, and the extract was cleaned up by solid phase extraction (SPE), separated on a DB-5 capillary column, ionized by electron impact and quantitated in the selective reaction monitor (SRM) mode. Good linearity was observed for all the analytes in the concentration ranges tested (0.04–2 mg/kg for phthalate acid esters, 1–40 mg/kg for diisodecyl phthalate (DINP), and 0.01–0.4 mg/kg for polycyclic aromatic hydrocarbons and polychlorinated biphenyls), with correlation coefficients more than 0.99. The limits of detection (LODs) were 8 μg/kg for DINP and 0.08–2 μg/kg for the other compounds. The recoveries ranged from 62.7% to 128.3%, with relative standard deviations (RSDs) of 1.1% to 13.6% (n = 6). The method was sensitive, accurate, simple, rapid and thus suitable for the detection of phthalate acid esters, polycyclic aromatic hydrocarbons and polychlorinated biphenyls in edible oils.

Key words: gas chromatography-tandem mass spectrometry, phthalates, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, edible oils

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