色谱

色谱

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气相色谱-质谱法同时测定动物内脏中的14种酞酸酯类环境激素残留

林竹光1,孙若男1,张莉莉1,邹西梅1,陈美瑜1,涂逢樟1,2,马玉1,蒋文静1   

  1. 1.Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University,The Key Laboratory of Analytical Sciences of the Ministry of Education, Xiamen 361005, China;
    2.Department of Chemistry and Material Engineering, Longyan College, Longyan 364000, China
  • 收稿日期:2007-09-19 修回日期:2007-12-13 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 林竹光

Simultaneous determination of 14 phthalate ester residues in animal innards by gas chromatography-mass spectrometry with electron impact ionization

LIN Zhuguang1, SUN Ruonan1, ZHANG Lili1, ZOU Ximei1, CHEN Meiyu1, TU Fengzhang1,2, MA Yu1, JIANG Wenjing1   

  1. 1.Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University,The Key Laboratory of Analytical Sciences of the Ministry of Education, Xiamen 361005, China;
    2.Department of Chemistry and Material Engineering, Longyan College, Longyan 364000, China
  • Received:2007-09-19 Revised:2007-12-13 Online:2008-05-30 Published:1984-03-25
  • Contact: LIN Zhuguang

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摘要： 开展了动物内脏中14种酞酸酯类（PAEs）环境激素残留的气相色谱-电子轰击离子源/质谱（GC-EI/MS）的分析方法研究。优化与选择了动物内脏样品的前处理条件，动物内脏样品经正己烷/二氯甲烷（1/1，v/v）混合提取剂超声提取、Florisil硅藻土固相萃取柱净化与乙酸乙酯/正己烷（2/3，v/v）混合洗脱剂洗脱和浓缩后，以邻苯二甲酸二苯基酯（DPhP）为内标物，采用GC-EI/MS的选择离子监测方式（SIM）进行定性和定量分析。当猪肝样品的加标浓度水平为100、200、400 μg/kg时，加标回收率为：60%~110%，相对标准偏差为：0.78%~10.3%；除邻苯二甲酸二（2-甲氧基乙基）酯（DMEP）与邻苯二甲酸二（2-乙氧基乙基）酯（DEEP）的检测限（MDL）分别为3.30与2.25 μg/kg外，其余的12种PAEs的MDL ≦ 1.74 μg/kg；线性范围为50 ~ 800 μg/kg，相关系数都大于0.9994。此分析方法成功地应用于6种动物内脏中14种痕量PAEs残留的分析。

关键词: 动物内脏, 气相色谱-电子轰击离子源质谱法, 酞酸酯

Abstract: An analytical multiresidue method was developed for the simultaneous determination of 14 phthalate esters (PAEs) in animal innards by gas chromatography-mass spectrometry with electron impact ionization (GC-EI/MS). After the optimization of different parameters such as the extraction solvent, PAEs were extracted from animal innards with hexane-dichloromethane (11, v/v) in an ultrasonic bath and cleaned up on a Florisil column, then were determined by GC-EI/MS in selected ion monitoring mode with diphenyl phthalate (DPhP) as internal standard. The recovery studies were performed at 100, 200 and 400 μg/kg levels for each PAE, and the recoveries ranged from 60%-110% with the relative standard deviations between 0.8% and 10.3% for different PAEs. The detection limit of the method was less than 1.74 μg/kg for most of PAEs except dimethoxyethyl phthalate (DMEP) and di(2-ethoxyethyl) phthalate (DEEP). The method was linear over the range of 50.0-800.0 μg/kg with the correlation coefficients larger than 0.9994. The method has been successfully applied to the determination of 14 PAEs in six animal innards.

Key words: animal innards, phthalate esters (PAEs) , gas chromatography-mass spectrometry with electron impact ionization (GC-EI/MS)