食品科学 ›› 2014, Vol. 35 ›› Issue (6): 125-128.doi: 10.7506/spkx1002-6630-201406026

• 分析检测 • 上一篇    下一篇

固相微萃取-气相色谱-质谱法测定食品塑料包装袋中6 种酞酸酯类化合物

陈德文,廖新艳,王正林,周 江,王国建   

  1. 国家日用小商品质量监督检验中心,浙江 义乌 322000
  • 收稿日期:2013-10-15 修回日期:2014-03-06 出版日期:2014-03-25 发布日期:2014-04-04
  • 通讯作者: 陈德文 E-mail:dewenc@hotmail.com
  • 基金资助:

    浙江省质量技术监督系统科研项目(20110239)

Determination of 6 Phthalate Esters in Food-Packaging Plastic Bags Using Solid-Phase Microextraction- Gas Chromatography-Mass Spectrometry

CHEN De-wen, LIAO Xin-yan, WANG Zheng-lin, ZHOU Jiang, WANG Guo-jian   

  1. National Center of Quality Supervision and Inspection for Commodity, Yiwu 322000, China
  • Received:2013-10-15 Revised:2014-03-06 Online:2014-03-25 Published:2014-04-04
  • Contact: CHEN De-wen E-mail:dewenc@hotmail.com

摘要:

建立固相微萃取-气相色谱-质谱同时测定食品塑料包装袋中6 种酞酸酯类化合物的分析方法,并对固相微萃取方式、萃取溶剂、萃取头涂层、萃取温度等参数进行优化。采用85 μm PA固相微萃取纤维头、正己烷为萃取溶剂,90 ℃平衡5 min后萃取吸附30 min,在250 ℃进样口解吸5 min后供气相色谱-质谱分析。结果表明:该方法的线性范围为0.25~50 mg/L,方法检出限为0.049~0.920 mg/L,回收率为82.2%~109.0%,相对标准偏差(n=6)为4.0%~12.0%,该方法能很好地富集基体中的目标化合物,满足食品塑料包装袋中多种酞酸酯类化合物的分析要求。

关键词: 固相微萃取, 气相色谱-质谱法, 食品塑料包装袋, 酞酸酯类化合物

Abstract:

A method based on solid-phase microextraction (SPME) technique followed by gas chromatography-mass
spectrometry (GC-MS) was developed for the determination of 6 phthalic acid esters (PAEs) in food-packaging plastic bags.
The parameters affecting the partitions of the analytes such as fiber coating, extraction temperature and extraction style were
optimized. The final SPME method employed an 85 μm polyacrylate (PA)-coating fiber and the extraction solvent used was
n-hexane. After equilibration for 5 minutes at 90 ℃, headspace adsorption for 30 minutes was carried out. Then the fiber
was introduced into the GC injector port and the extract was desorbed at 250 ℃ for 5 min. The linear range of the method
was 0.25-50 mg/L. The detection limits for 6 PAEs were in the range of 0.049?0.920 mg/L, and the recoveries from spiked
samples were 82.2%?109.0% with RSDs (n = 6) of 4.0%?12.0%. The method enables enrichment of PAEs from sample
matrices and can meet the requirements for the analysis of PAEs in food-packaging plastic bags.

Key words: solid-phase microextraction (SPME), gas chromatography-mass spectrometry (GC-MS), food-packaging plastic bag, phthalic acid esters (PAEs)

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