食品科学

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气相色谱-质谱/质谱法同时测定硅橡胶餐具中21种硅氧烷类化合物的残留量

董犇1,张子豪2,曾莹2,王 晶1,钟怀宁3,廖满生4,郑建国2,5,刘中勇6,陈胜1,李丹2   

  1. 1. 广东海关技术中心
    2. 广州海关技术中心
    3. 广东出入境检验检疫局检验检疫技术中心
    4. 中国检验认证集团广东有限公司
    5.
    6. 广东检验检疫技术中心
  • 收稿日期:2020-12-18 修回日期:2021-03-18 出版日期:2021-04-13 发布日期:2021-04-13
  • 通讯作者: 李丹
  • 基金资助:
    重要贸易产品技术性贸易措施应对检测评价技术研究;进口新型食品接触材料中新发安全因子的非靶向筛查与检测技术研究

Simultaneous determination of the residues of 21 kinds of siloxane compounds in silicone tableware by Gas Chromatography-mass/mass spectrometry

  • Received:2020-12-18 Revised:2021-03-18 Online:2021-04-13 Published:2021-04-13
  • Contact: 李 丹

摘要: 硅氧烷及其低聚物残留成为食品接触材料新的风险关注点,为有效考察食品硅橡胶餐具中硅氧烷类化合物的残留量,采用气相色谱-质谱/质谱法(GC-MS/MS)建立了同时测定硅橡胶餐具中21种硅氧烷类化合物残留量的方法。对用乙酸乙酯提取后的样品中21种硅氧烷类化合物以ZB-5HT(15 m × 0.25 mm × 0.1 μm)色谱柱进行分离,采用电喷雾离子源(ESI),多反应监测(MRM)模式进行扫描。结果表明,21种硅氧烷类化合物的色谱分离效果良好,在0.05~2.50 mg/L浓度范围内线性关系良好,最低检出限除三甲基三苯基环三硅氧烷、四甲基四苯基环四硅氧烷和五甲基五苯基环五硅氧烷为0.20 mg/kg,其余化合物均为 0.05 mg/kg。加标回收率在91.3%~107.8%之间,相对标准偏差均低于5.0%。该方法快速高效、线性范围好,适用于硅橡胶餐具中21种硅氧烷类化合物残留量的检测。

关键词: 硅橡胶食品接触材料, 硅氧烷类化合物, 气相色谱-质谱/质谱法(GC-MS/MS)

Abstract: Siloxane and its oligomer residues have become a new risk concern for food contact materials. In order to evaluate the residues of 21 kinds of siloxane compounds in food tableware, a method for the simultaneous determination of 21 siloxane compounds in tableware was established by GC-MS/MS. The 21 siloxane compounds in the extracted samples were separated by ZB-5HT (15 m × 0.25 mm × 0.1 m) chromatographic column and scanned by multi-reaction monitoring (MRM) mode using electrospray ion source (ESI). The results showed that 21 kinds of anti-siloxane compounds had good chromatographic separation effect and good linear relationship in the concentration range of 0.05 - 2.50 mg/L. The minimum detection limit was 0.20 mg/kg except for trimethyltriphenylcyclotrisiloxane, tetramethyltetraphenylcyclopentasiloxane and pentamethylpentaphenylcyclopentasiloxane, and the remaining compounds were all 0.05 mg/kg. The standard recovery was 91.3%-107.8%, and the relative standard deviation was lower than 5.0%. The method is fast, efficient and has a good linear range. It is suitable for the determination of 21 kinds of siloxane residues in silicone rubber tableware.

Key words: silicone rubber food contact materials, siloxane compounds, gas chromatography-mass/mass spectrometry (GC-MS/MS)

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