食品科学

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超声辅助萃取-大体积进样在线衍生-气相色谱串联质谱法测定食品中的苯甲酸

国 明,李祖光,王 芳,聂 晶,魏 丹   

  1. 浙江工业大学化学工程与材料学院,浙江 杭州 310014
  • 出版日期:2013-12-25 发布日期:2014-01-03

Determination of Benzoic Acid in Foods by Sonication-Assisted Extraction and Gas Chromatography-Tandem Mass Spectrometry with Large-Volume Online Derivatization

GUO Ming,LI Zu-guang,WANG Fang,NIE Jing,WEI Dan   

  1. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China
  • Online:2013-12-25 Published:2014-01-03

摘要:

建立超声辅助萃取-大体积进样在线衍生-气相色谱串联质谱测定食品中苯甲酸含量的方法。采用乙腈为提取剂进行超声萃取,经离心分离后,以四丁基硫酸氢铵为衍生化试剂进行衍生,利用直接进样杆装置在气相色谱进样口进行在线衍生以提高分析灵敏度,采用DB-5MS毛细管色谱柱,通过气相色谱-离子阱串联质谱进行分析测定。结果表明:苯甲酸在0.50~10.0μg/mL范围内线性关系良好(r=0.9976),方法的检出限和定量限分别为12.8ng/mL和42.7ng/mL。本方法具有操作简单、无需净化步骤、准确度高、重复性好等优点,可适用于食品中苯甲酸含量的测定。

关键词: 苯甲酸, 气相色谱串联质谱, 在线衍生, 四丁基硫酸氢铵, 超声辅助萃取

Abstract:

A method using sonication-assisted extraction for quantitatively determining benzoic acid in foods was
established by gas chromatography-tandem mass spectrometry (GC-MS-MS) with large-volume online derivatization
samples were extracted with acetonitrile, and then centrifugated. The supernatant was added with tetrabutylammonium
hydrogen sulfate (TBAHS) as a derivatization reagent while magnetic stirring. The method used gas chromatography
with ChromatoProbe for on-line derivatization to improve sensitivity. Analysis was performed on a DB-5MS capillary
column supplemented with GC-ion trap tandem mass spectrometry. The calibration curves of the analyte revealed a
good linear relationship over the range of 0.50–10.0 μg/mL (r = 0.9976). The limit of detection (LOD) and limit
of quantitation (LOQ) of the developed method were 12.8 ng/mL and 42.7 ng/mL, respectively. This method has
the advantages of convenient operation, no need for purification, high sensitivity, excellent accuracy and good
reproducibility and thus, is suitable for the determination of benzoic acid in food samples.

Key words: benzoic acid, gas chromatography-tandem mass spectrometry (GC-MS-MS), online derivatization, tetrabutylammonium hydrogen sulfate (TBAHS), sonication-assisted extraction