色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 21-26.DOI: 10.3724/SP.J.1123.2018.09002

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

正化学源-气相色谱-质谱法测定食用植物油中有机锡化合物残留

王红1, 沈伟健1, 吴斌1, 余可垚1, 姜珊1, 陆慧媛1, 胡国绅1, 王毅谦1, 高玲1, 宋杰铭2   

  1. 1. 南京海关动植物与食品检测中心, 江苏 南京 210019;
    2. 南京市第一中学, 江苏 南京 210001
  • 收稿日期:2018-08-31 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 沈伟健,Tel:(025)52345193,E-mail:45467447@qq.com.
  • 基金资助:

    南京海关科技计划项目（2018KJ38，2017KJ05）.

Determination of organo-tin residues in edible vegetable oil by positive chemical ionization-gas chromatography-mass spectrometry

WANG Hong1, SHEN Weijian1, WU Bin1, YU Keyao1, JIANG Shan1, LU Huiyuan1, HU Guoshen1, WANG Yiqian1, GAO Ling1, SONG Jieming2   

  1. 1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China;
    2. Nanjing No.1 Middle school, Nanjing 210001, China
  • Received:2018-08-31 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Nanjing Customs Research Project (Nos. 2018KJ38, 2017KJ05).

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摘要：

建立了正化学源-气相色谱-质谱技术测定食用植物油中有机锡化合物残留的方法。食用油样品经环己烷-乙酸乙酯（1：1，v/v）溶解后，经凝胶渗透色谱（GPC）净化，目标馏分用四乙基硼酸钠进行衍生。采用基质校正曲线外标法定量，在20~2000 μg/L范围内，7种有机锡化合物均呈现良好的线性关系，相关系数大于0.99，定量限为0.3~1.2 μg/kg。对芝麻油样品进行加标回收试验，在0.05、0.10、0.20 mg/kg 3个添加水平下，7种有机锡化合物的平均回收率为66.2%~103.2%，相对标准偏差均小于11.5%。该方法精密度好，灵敏度高，可用于食用植物油中有机锡化合物残留量的测定。

关键词: 气相色谱-质谱, 食用植物油, 有机锡, 正化学源

Abstract:

For the determination of organo-tin residues in edible vegetable oil, a method was developed based on gas chromatography-mass spectrometric (GC-MS) with positive chemical ionization (PCI). The edible oil samples were first dissolved by cyclohexane-ethyl acetate (1:1, v/v), and then purified by gel permeation chromatography (GPC). After derivatization by sodium tetraethylborate, the samples were analyzed by GC-MS with PCI source in the single ion monitor (SIM) mode. The seven organo-tin compounds showed good linear relationships in the range of 20-2000 μg/L and the correlation coefficients exceeded 0.99. The limits of quantitation (LOQs) and the average recoveries of the seven organo-tin compounds were 0.3-1.2 μg/kg and 66.2%-103.2%, respectively, and the relative standard deviations were less than 11.5% at three spike levels (0.05, 0.10, and 0.20 mg/kg). The method showed good linearity and high sensitivity and can be used for the determination of organo-tin residues in edible vegetable oil.

Key words: edible vegetable oil, gas chromatography-mass spectrometry (GC-MS), organo-tin, positive chemical ionization (PCI)

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