色谱

色谱

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微滴液相微萃取技术用于气相色谱-质谱法测定食品中的酞酸酯

李玫瑰,李元星,毛丽秋   

  1. Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha 410081, China
  • 收稿日期:2006-04-05 修回日期:2006-06-15 出版日期:2007-01-30 发布日期:1986-03-25
  • 通讯作者: 毛丽秋

Application of Single Drop Microextraction in the Determination of Phthalate Esters in Food by Gas Chromatography-Mass Spectrometry

LI Meigui, LI Yuanxing, MAO Liqiu   

  1. Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha 410081, China
  • Received:2006-04-05 Revised:2006-06-15 Online:2007-01-30 Published:1986-03-25
  • Contact: MAO Liqiu

PDF

956

被引次数

155

摘要： 将一种新型、简单、快速、环境友好的萃取方法微滴液相微萃取(SDME)与气相色谱-质谱法结合用于快速分析食品中的几种酞酸酯(PAEs)。考察了萃取溶剂的种类及用量、微液滴在样品溶液中的深度、萃取时间及搅拌子的搅拌速度对微滴液相微萃取的影响。优化的萃取条件为:萃取溶剂为2.0 μL甲苯,微液滴在样品溶液中的深度为0.75 cm,搅拌速度为1000 r/min,萃取时间为20 min。该方法的线性范围为0.1～4000 μg/L,检测限为25 ng/L～0.8 mg/L,加标回收率为87.1%～114.4%,相对标准偏差为4.9%～11.6%。微滴液相微萃取所需的有机溶剂量很小，是一种快速、简单、安全、有效的水溶性样品的前处理方法。

关键词: 气相色谱-质谱法, 食品 , 酞酸酯, 微滴液相微萃取

Abstract: A novel, simple, fast and environment-friendly method based on single drop microextraction (SDME) was developed for the determination of phthalate esters in food by gas chromatography-mass spectrometry (GC-MS). The effects of the nature of organic solvents, microdrop volume, the depth of microdrop in sample solution, extration time and stirring rate on the extraction efficiency were investigated separately. The optimal SDME conditions, 2.0 μL of toluene, 0.75 cm of the depth of microdrop, 1000 r/min of stirring rate and 20 min of extraction time, were obtained and used for the analysis of dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), dioctyl phthalate (DOP) and diethylhexyl phthalate (DEHP) in food. At first, a sample was dissolved with de-ionized water and then extracted with ultrasonication for 15 min. Then, it was filtrated and the solution was extracted and concentrated by a single drop of a solvent. Finally, it was analyzed by GC-MS. The reproducibility, linearity, recovery, and limit of detection of the method were studied. The results showed that the limits of detection (LOD) were between 25 ng/L and 0.8 mg/L. The overall recoveries were 87.1%114.4% with the relative standard deviations of 4.9%11.6%. This method has been successfully applied to the analysis of food samples.

Key words: food , gas chromatography-mass spectrometry (GC-MS), phthalate esters (PAEs), single drop microextraction (SDME)