色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 27-32.DOI: 10.3724/SP.J.1123.2011.08019

• 研究论文 • 上一篇    下一篇

固相萃取-气相色谱-质谱法测定食品中23种邻苯二甲酸酯

郑向华1, 林立毅1, 方恩华1, 黄永辉2, 周爽1, 周昱1, 郑小严2, 徐敦明1*   

  1. 1. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361026; 2. 福建省产品质量检验研究院, 福建 福州 350002
  • 收稿日期:2011-08-15 修回日期:2011-09-23 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 徐敦明,博士,高级工程师,主要从事食品安全分析. Tel: (0592)3269935,
  • 基金资助:
    国家质检总局行业标准制修订计划项目(2011B341J)和厦门出入境检验检疫局科技项目(2011XK005).

Determination of 23 phthalate esters in food by solid-phase extraction coupled with gas chromatography-mass spectrometry

ZHENG Xianghua1, LIN Liyi1, FANG Enhua1, HUANG Yonghui2, ZHOU Shuang1, ZHOU Yu1, ZHENG Xiaoyan2, XU Dunming1*   

  1. 1. Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China; 2. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China
  • Received:2011-08-15 Revised:2011-09-23 Online:2012-01-28 Published:2012-03-01

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935

被引次数

230

摘要： 建立了同时检测食品中23种邻苯二甲酸酯类化合物的固相萃取-气相色谱-质谱(GC-MS)分析方法。样品经正己烷或乙腈提取、玻璃ProElut PSA固相萃取柱净化,GC-MS选择离子监测模式(SIM)测定。考察了不同种类食品的提取、净化方法。23种邻苯二甲酸酯的线性范围除邻苯二甲酸二异壬酯(DINP)和邻苯二甲酸二异癸酯(DIDP)为0.5～5 mg/L外,其余均为0.05～5 mg/L,相关系数(r)除DIDP外均大于0.99。方法的检出限(信噪比为3)为0.005～0.05 mg/kg,定量限(信噪比为10)为0.02～0.2 mg/kg。在10种食品基质中3个加标水平的平均回收率为77%～112%,相对标准偏差(RSD,n=6)为4.1%～12.5%。该方法稳定、可靠,操作简单,适用于食品中邻苯二甲酸酯类化合物的检测与确证。

关键词: 固相萃取, 邻苯二甲酸酯, 气相色谱-质谱, 食品, 增塑剂

Abstract: A method for the simultaneous determination of 23 phthalate esters in food samples by solid-phase extraction coupled with gas chromatography-mass spectrometry (SPE-GC-MS) was developed and evaluated. The samples were extracted with hexane or acetonitrile, and cleaned up with a glass ProElut PSA SPE column. The identification and quantification were performed by GC-MS in selected ion monitoring (SIM) mode. The extraction processes of different foods were investigated. The calibration curves of phthalate esters showed good linearity in the range of 0.05~5 mg/L (0.5~5 mg/L for diisononyl phthalate (DINP), diisodecyl-phthalate (DIDP)) with the correlation coefficients (r) between 0.9848 and 0.9996. The limits of detection of phthalate esters in food samples ranged from 0.005 to 0.05 mg/kg (S/N=3) and the limits of quantification ranged from 0.02 to 0.2 mg/kg (S/N=10). The average recoveries of 23 analytes spiked in 10 kinds of food matrices ranged from 77% to 112% with the relative standard deviations (RSDs, n=6) of 4.1%~12.5%. The method is suitable for the determination of 23 phthalate esters simultaneously in foodstuffs with easy operation, high accuracy and precision.

Key words: gas chromatography-mass spectrometry (GC-MS), foods, phthalate esters (PAEs), plasticizer, solid-phase extraction (SPE)