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.pdf

※分折检
品学
2013,WU.34,Mo.24197
超声辅助萃取-大体积进样在线衍生气相色谐
串联质谱法测定食品中的苯中酸
国明,李祖光“,王芳,聂品,魏丹
浙江工业大学化学工程与材料学院,浙江杭州310014)
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。采用乙腊为提
取剂进行超声萃取,经离心分离后,以四丁基疏酸氢铵为行生化试剂进行衍生,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0.50~10.0gmL范圃内线性关系良好(=0.976),方法的检出限和定量限分别为12.8 ng/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
关闹:苯甲酸;气相色谱串联质谱;在线衍生;四丁基硫酸氢铵;超声輔助萃取
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
(College of hemical Engineering and Materials Science, Zhejang University of Technology, Hangzhou 310014, China)
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 hromatoprobe for on-line derivatization o improve sen itiit 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/ml(=0.9976). The limit of detection(L,OD)and limit
of quantitation ( L0Q of the developed method were 12.8 ng/ML and 42.7 ng/ml, respectivcly. 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-asisted extraction
中图分类号:065763
文献标志码:A
文章编号:1002-6630(2013)24-0197-05
doi:l0.75066pix100-6630201324041
作为最低级芳香族一元酸,苯甲酸对多种微生物细长食品的保质期,在调味食品生产领域被广泛应用,但食
胞呼吸騂系的活性有抑制作用,对于阻得乙酰辅酶A的品添加剂过量摄入后必然会影响人体的健康叩。近年来,
结合反应具有较强的作用,并对微生物的细胞膜有阻碍苯甲酸逐渐成为食品安全的研究热点问题。目前,检测苯
作用。因此,苯甲酸既能抑制微生物的生长繁殖,又具甲酸的常用方法有高效液相色谱法Pり、气相色谱法
有良好的杀菌作用,可以作为食品中理想的防腐剂,延气相色谱-质谱法Pリ。对于成分复杂的食品样品,高效
收稿日期:2012-12-21
基金项目:浙江省科技厅钱江人才基金資助项目(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韓登项目(Pd2013016):浙江省重点创新团队项目(2010R5001806
作者简介:国明(1988-),男,硕士研究生,研究方向为分析化学。E-mail:guoming107@126.com
通信作者:李祖光(1971-),男,教授,博士,研究方向为分析化学。E-mail:lzg@zjut.edu.cn
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