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  

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

作　　者：国明[1] 李祖光[1] 王芳[1] 聂晶[1] 魏丹[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310014

出　　处：《食品科学》2013年第24期197-201,共5页Food Science

基　　金：浙江省科技厅钱江人才基金资助项目(2010R10044);国家人力资源与社会保障部2011年度留学人员科技活动择优资助(优秀类)项目(2011443);浙江省本科院校中青年学科带头人学术攀登项目(Pd2013016);浙江省重点创新团队项目(2010R50018-06)

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0．50～10．0／ag／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。A method using sonication-assisted extraction for quantitatively determining benzoic acid in tbods 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-SMS 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.

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 

分 类 号：O657.63[理学—分析化学]