色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 733-737.DOI: 10.3724/SP.J.1123.2012.03002

• 技术与应用 • 上一篇    下一篇

气相色谱-质谱法测定软木塞中2种霉味物质

唐熙1, 梁鸣1, 李小晶1*, 熊文明2, 唐泓1, 姜晓黎1, 陈佳敏1   

  1. 1. 福建出入境检验检疫局技术中心, 福建 福州 350001; 2. 福州大学化学化工学院, 福建 福州 350002
  • 收稿日期:2012-03-01 修回日期:2012-04-15 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 李小晶,博士,高级工程师,主要从事食品及食品接触材料中有毒有害物质的检测研究. E-mail: lxjciq@hotmail.com.
  • 基金资助:

    福建省科技计划重点项目(2011Y0001)和国家质量监督检验检疫总局科技计划项目(2011IK028).

Determination of two mouldy compounds in cork by gas chromatography-mass spectrometry

TANG Xi1, LIANG Ming1, LI Xiaojing1*, XIONG Wenming2, TANG Hong1, JIANG Xiaoli1, CHEN Jiamin1   

  1. 1. Technology Center of Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China; 2. College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350002, China
  • Received:2012-03-01 Revised:2012-04-15 Online:2012-07-28 Published:2012-07-19

PDF

362

被引次数

5

摘要： 建立了一种简便、快速的可同时测定软木塞中两种霉味物质(2,4,6-三氯苯甲醚(TCA)和2,4,6-三溴苯甲醚(TBA))的气相色谱-质谱联用(GC-MS)方法。软木塞样品采用甲醇超声萃取,N-丙基乙二胺(PSA)固相萃取柱净化,浓缩后采用GC-MS进行分析,外标法定量。在10～10000 μg/L的质量浓度范围内,TCA和TBA均有较好的线性关系,相关系数(r2)大于0.99。通过对不同种类的软木塞空白样品进行加标回收率试验和精密度试验考察方法的可行性。结果表明TCA和TBA的回收率介于88.4%与97.6%之间,相对标准偏差介于1.02%与4.58%之间。TCA和TBA的检出限分别为12 μg/L和18 μg/L,定量限分别为40 μg/L和50 μg/L。本方法适用于市售瓶装葡萄酒软木塞中TCA和TBA的检测。

关键词: 2,4,6-三氯苯甲醚, 2,4,6-三溴苯甲醚, 气相色谱-质谱法, 软木塞

Abstract: A simple and fast method for the simultaneous determination of two mouldy compounds, 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA), in cork by gas chromatography-mass spectrometry (GC-MS) was established. The analytes were extracted by ultrasonic extraction with methanol, and purified then by solid phase extraction using primary secondary amine (PSA) as solid phase. After concentrating, the sample was analyzed by GC-MS and quantified by the external standard method. The linear ranges were from 10 μg/L to 10000 μg/L for TCA and TBA, the correlation coefficients (r2) of the calibration curves were above 0.99. The recoveries and the relative standard deviations (RSDs) of TCA and TBA in different kinds of corks were investigated. The recoveries ranged from 88.4% to 97.6% with the RSDs between 1.02% and 4.58% (n=6). The limits of detection (LODs) were 12 μg/L for TCA and 18 μg/L for TBA, and the limits of quantification (LOQs) were 40 μg/L for TCA and 50 μg/L for TBA. The method is suitable to the determination of TCA and TBA in corks.

Key words: 2,4,6-tribromoanisole (TBA), 2,4,6-trichloroanisole (TCA), cork, gas chromatography-mass spectrometry (GC-MS)