食品科学

• 分析检测 • 上一篇    下一篇

GC-MS法检测谷类、根茎类蔬菜中24种邻苯二甲酸酯

郭浩楠,凌 云,李玉玉,储晓刚   

  1. 中国检验检疫科学研究院食品安全研究所,北京 100025
  • 出版日期:2013-08-25 发布日期:2013-09-03

Determination of 24 Phthalate Ester Plasticizers in Cereals and Root Vegetables by Gas Chromatography-Mass Spectrometry

GUO Hao-nan,LING Yun,LI Yu-yu,CHU Xiao-gang   

  1. Food Safety Institute, Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Online:2013-08-25 Published:2013-09-03

摘要:

建立气相色谱-质谱法同时测定谷类、根茎类蔬菜中24种邻苯二甲酸酯的方法。样品经正己烷-水或者正己烷-丙酮-水提取,正己烷层浓缩至干后定容,气相色谱-质谱联用仪测定,内标法定量。方法具有良好线性,相关系数r均大于0.999,检测限在0.001~0.1mg/kg之间,平均回收率在78.7%~113.2%范围内,相对标准偏差为0.4%~14.4%。采用该方法对国内市售谷类、根茎类蔬菜中邻苯二甲酸酯进行检测,实际样品中检出了邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二(2-乙基己)酯和邻苯二甲酸二异壬酯等。此方法可满足目前谷类、根茎类蔬菜中邻苯二甲酸酯的检测要求。

关键词: 邻苯二甲酸酯, 气相色谱-质谱法, 谷类, 根茎类蔬菜

Abstract:

A method for simultaneous determination of 24 phthalate acid esters (PAEs) in cereals and root vegetables
was developed. Samples were extracted by n-hexane/distilled water or n-hexane/acetone/distilled water. The collected
supernatants were vacuum-concentrated to dryness and re-dissolved in n-hexane. PAEs were measured by gas
chromatography-mass spectrometer (GC-MS) using internal standard method. The correlation coefficients (r) of 24 PAEs
were over 0.999 with detection limits between 0.001 mg/kg and 0.1 mg/kg. The average recoveries of 24 PAEs in cereals
and root vegetables varied from 78.7% to 113.2%, with relative standard deviations (RSDs) between 0.4% and 14.4%. The
migration amount of PAEs plasticizers in cereals and root vegetables was investigated by this method, diethyl phthalate,
di-n-butyl phthalate, di-2-ethylhexyl phthalate and di-iso-nonyl phthalate were found in some commercial samples. This
method is well suitable for the analysis of PAEs in cereals and root vegetables.

Key words: phthalate acid esters, gas chromatography-mass spectrometry (GC-MS), cereal, root vegetables