色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1236-1239.DOI: 10.3724/SP.J.1123.2011.01236

• 技术与应用 • 上一篇    下一篇

凝胶渗透色谱净化-高效液相色谱法测定油脂食品中的邻苯二甲酸酯类增塑剂

张春雨1, 王辉2, 张晓辉1, 马忠强1, 邓宛梅1, 胡克1, 丁明玉2*   

  1. 1. 北京莱伯泰科有限公司, 北京 101312; 2. 清华大学化学系, 北京 100084
  • 收稿日期:2011-08-17 修回日期:2011-09-27 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 丁明玉,博士,教授,主要从事色谱领域的研究
  • 基金资助:

    国家自然科学基金项目（No. 21075074）.

Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up

ZHANG Chunyu1, WANG Hui2, ZHANG Xiaohui1, MA Zhongqiang1, DENG Wanmei1, HU Ke1, DING Mingyu2*   

  1. 1. Beijing Labtech Group, Beijing 101312, China; 2. Department of Chemistry, Tsinghua University, Beijing 100084, China
  • Received:2011-08-17 Revised:2011-09-27 Online:2011-12-28 Published:2012-01-15
  • Contact: Ming-Yu DING

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973

被引次数

76

摘要： 建立了油脂食品(方便面、油炸糕点、沙琪玛、食用油等)中5种主要邻苯二甲酸酯类增塑剂的凝胶渗透色谱（GPC）净化-高效液相色谱(HPLC)分析方法。食品样品用石油醚超声提取,经GPC净化后,采用反相HPLC进行分析。所用的分离柱为Labtech C18(250 mm×4.6 mm, 5 μm),以乙腈和水为流动相,梯度洗脱。方法的相关系数皆在0.997以上,目标物的检出限(信噪比为3计)为3.25～13.4 μg/L。在50 mg/L添加水平时,目标物的加标回收率为70.4%～113.6%,相对标准偏差为0.3%～5.8%(n=3)。该方法简便、快捷、实用,可用于油脂食品中邻苯二甲酸酯类增塑剂的分析测定。

关键词: 高效液相色谱, 邻苯二甲酸酯, 凝胶渗透色谱, 增塑剂；油脂食品

Abstract: A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm×4.6 mm, 5 μm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25~13.4 μg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n=3) of 0.3%~5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

Key words: grease food, high performance liquid chromatography (HPLC), phthalates, plasticizers, gel permeation chromatography (GPC)