食品科学

• 分析检测 • 上一篇    下一篇

在线凝胶渗透色谱-气相色谱-质谱法测定食用油中20种邻苯二甲酸酯类物质

凌 云,贾 玮,蒋萍萍,黄峻榕,储晓刚   

  1. 1.中国检验检疫科学研究院,北京 100123;2.陕西科技大学生命科学与工程学院,陕西 西安 710021
  • 出版日期:2013-08-25 发布日期:2013-09-03

Rapid Determination of 20 Phthalate Acid Esters in Edible Oil by Online Gel Permeation Chromatography Coupled with Gas Chromatography-Mass Spectrometry

LING Yun,JIA Wei,JIANG Ping-ping,HUANG Jun-rong,CHU Xiao-gang   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    2. College of Life Science and Engineering, Shaanxi University of Science and Technology, Xi’an 710021, China
  • Online:2013-08-25 Published:2013-09-03

摘要:

建立测定食用油中20种邻苯二甲酸酯的在线凝胶渗透色谱串联气相色谱-质谱(GPC-GC-MS)分析方法。采用样品稀释后直接进行GPC-GC-MS方法分析,外标法定量。20种邻苯二甲酸酯类化合物在2.5~10000μg/L范围内具有较好的线性关系,相关系数均大于0.99。化合物在3个加标水平(LOQ、2LOQ、4LOQ)条件下的回收率在83%~118%范围内;方法的定量限LOQ(RSN≥10)范围为0.11~4.59mg/kg;相对标准偏差为1.9%~6.7%。该方法样品前处理简单、分析时间短、灵敏、可靠,适用于食用油中多种邻苯二甲酸酯类化合物的检测。

关键词: 在线凝胶渗透色谱串联气相色谱-质谱, 食用油, 邻苯二甲酸酯

Abstract:

A method was proposed for the rapid determination of 20 phthalate acid esters (PAEs) in edible oil based
on automated online gel permeation chromatography coupled with gas chromatograph-mass spectrometry (GPC-GCMS).
Diluted oils were directly determined by GPC-GC-MS. Identification and detection were achieved using electron impact (EI)
ionization in the selected ion monitoring (SIM) mode. The calibration curves of 20 PAEs were linear in the range of 2.5–10000 μg/L
with good correlation coefficients more than 0.99. The recoveries for all these compounds from edible oil at the spiked levels
of 1LOQ, 2LOQ and 4LOQ were in the range of 83%–118%. The limits of quantitation (RSN ≥ 10) for the PAEs were in the
range of 0.11–4.59 mg/kg and RSD were 1.9%–6.7%. The established method was successfully used for the determination
of real samples (bean oil, corn oil, sunflower oil, peanut oil and olive oil) from supermarkets. The method was simple, rapid
and reliable, and could meet the requirement for simultaneous determination and analysis of 20 PAEs in edible oil.

Key words: on-line gel permeation chromatography coupled with gas chromatography-mass spectrometry (GPC-GC-MS), edible oil, phthalate acid esters (PAEs)