色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 951-956.DOI: 10.3724/SP.J.1123.2012.05024

• 研究论文 • 上一篇    下一篇

在线富集-微乳液毛细管电动色谱法分析食品塑料袋中邻苯二甲酸酯类化合物

肖佳1, 黄颖1*, 王敏毅2, 陈国南3   

  1. 1. 福建师范大学化学与化工学院, 福建 福州 350007; 2. 福州职业技术学院技术工程系, 福建 福州 350108; 3. 福州大学 食品安全分析与检测教育部重点实验室, 福建 福州 350002
  • 收稿日期:2012-05-18 修回日期:2012-07-03 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 黄颖,博士,教授,主要研究方向为电分析化学与毛细管电泳. E-mail: huangying@fjnu.edu.cn.
  • 基金资助:

    福建省属高校科研专项基金项目(JK2010008)、福建省教育厅项目（JA09282）、福州大学食品安全分析与检测教育部重点实验室开放基金项目(FS11003)、福建师范大学本科生课外科技计划项目(BKL2010-026)和福建省大学生创新性实验计划项目(Fjnu2010-006).

Analysis of phthalate esters in plastic-packaging bags by on-line sample stacking-microemulsion electrokinetic chromatography

XIAO Jia1, HUANG Ying1*, WANG Minyi2, CHEN Guonan3   

  1. 1. College of Chemistry and Chemical Engineering, Fujian Normal University, Fuzhou 350007, China; 2. Department of Technology and Engineering, Fuzhou Polytechnic, Fuzhou 350108, China; 3. Key Laboratory of Analysis and Detection for Food Safety, Ministry of Education, Fuzhou University, Fuzhou 350002, China
  • Received:2012-05-18 Revised:2012-07-03 Online:2012-09-28 Published:2012-09-20

PDF

337

被引次数

7

摘要： 建立了微乳液毛细管电动色谱(MEEKC)模式下,采用常规样品堆积模式(normal stacking mode, NSM)和反向极性堆积模式(reversed electrode polarity stacking mode, REPSM)两种在线富集邻苯二甲酸酯类化合物(phthalate esters, PAEs)的简便、有效方法。与常规MEEKC方法相比,REPSM-MEEKC方法使4种PAEs的检测灵敏度提高了937.5～7143倍。考察了常规MEEKC的分离条件,分别对影响两种富集过程的一些因素进行了研究,同时对两种富集方法的重现性和检出限等进行了考察。NSM-MEEKC和REPSM-MEEKC对邻苯二甲酸酯类化合物的检出限(按信噪比(S/N)=3计)分别为0.021～0.33 mg/L和0.7～4 μg/L。其中,灵敏度更高的REPSM-MEEKC方法已成功应用于食品塑料袋中邻苯二甲酸酯类化合物的测定,加标回收率为89.1%～105.6%,结果令人满意。

关键词: 常规样品堆积, 反向极性堆积, 邻苯二甲酸酯类化合物, 塑料袋, 微乳液毛细管电动色谱

Abstract: Two convenient, effective, and reproducible methods using microemulsion electrokinetic chromatography (MEEKC)-normal stacking mode (NSM) and reversed electrode polarity stacking mode (REPSM) were developed for the on-line sample stacking of phthalate esters (PAEs). REPSM coupled with MEEKC increased the sensitivity of 937.5 to 7143 times for four PAEs compared to the conventional MEEKC. The separating conditions in the MEEKC method were studied, and many factors influencing the two sample stacking processes were investigated in detail. The optimum sample matrices for the two stacking methods were as follows: 30 mmol/L sodium cholate (SC) and 30.0 mmol/L borate (pH 8.5). Additionally, sample injections as large as 3.45 kPa×40 s and 3.45 kPa×90 s were applied for NSM-MEEKC and REPSM-MEEKC, respectively. The linear relationship and reproducibility were also examined. Under the optimum conditions, the detection limits (S/N=3) of the PAEs were in the ranges of 0.021~0.33 mg/L and 0.7~4 μg/L for NSM-MEEKC and REPSM-MEEKC, respectively. The proposed REPSM-MEEKC has been successfully applied to determine PAEs in plastic-packaging bags, and the spiked recoveries were in the range of 89.1%~105.6% with satisfactory results.

Key words: normal stacking mode, phthalate esters, plastic-packaging bags, reversed electrode polarity stacking mode, microemulsion electrokinetic chromatography

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