色谱

色谱

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顶空固相微萃取-气相色谱-质谱法快速测定酱油中的挥发性风味成分

严留俊,张艳芳,陶文沂,王利平,吴胜芳

  

  1. Key Laboratory of Industrial Biotechnology, Ministry of Education, Jiangnan University, Wuxi 214122, China
  • 收稿日期:2007-09-03 修回日期:2007-12-11 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 陶文沂

Rapid determination of volatile flavor compounds in soy sauce using head space solid-phase microextraction
and gas chromatography-mass spectrometry

YAN Liujun, ZHANG Yanfang, TAO Wenyi, WANG Liping, WU Shengfang

  

  1. Key Laboratory of Industrial Biotechnology, Ministry of Education, Jiangnan University, Wuxi 214122, China
  • Received:2007-09-03 Revised:2007-12-11 Online:2008-05-30 Published:1984-03-25
  • Contact: wytao1946@163.com

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摘要：

建立了一种快速简便地测定酱油中挥发性风味成分的顶空固相微萃取（HS-SPME）-气相色谱-质谱法(GC-MS)。以2-辛醇为内标,考察了萃取头、萃取时间、离子强度、萃取温度对酱油样品中挥发性风味物质萃取的影响。该方法对酱油中常见挥发性风味成分的测定有良好的重复性和回收率,对常见挥发性物质的定量比较准确。优化的HS-SPME条件为：涂层厚度为85 μm聚丙烯酸酯(PA)萃取纤维头,于45 ℃、NaCl质量浓度为250 g/L下对酱油样品顶空吸附40 min,于250 ℃下解吸2 min后进行GC-MS分离鉴定。酱油样品的分析结果表明,其挥发性风味物质中含量较高的是醇、酸、酯和酚类,此外还有一些羰基化合物和杂环化合物。

关键词: 顶空固相微萃取, 挥发性风味成分, 酱油 , 气相色谱-质谱法

Abstract:

A rapid and simple method was developed for the determination of volatile flavor compounds (VFCs) in soy sauce by head space solid-phase microextraction (HS-SPME) coupled to capillary gas chromatography-mass spectrometry (GC-MS). Five types of SPME fibers, including 85 μm PA, 100 μm PDMS, 75 μm CAR/PDMS, 65 μm PDMS/DVB, 50 μm DVB/CAR/PDMS were investigated. Three parameters for HS-SPME in terms of adsorption time, salt concentration, and extraction temperature were optimized. Adsorption time tested in this study were 20, 40 and 60 minutes; the salt concentrations were 180, 210, 250, 270 and 300 g/L; and extraction temperatures were 25, 35, 45, 55 and 65 ℃. The concentrations of the compounds were calculated based on their relative peak areas to the internal standard of 2-octanol. An 85 μm PA fiber, adsorption time of 40 min, a temperature of 45 ℃ and NaCl concentration of 250 g/L were selected as th optimum conditions. This optimized method was applied to evaluate a real sample. As a result, 97 compounds in a soy sauce sample were isolated and identified successfully. The results showed that alcohols, carboxylic acids, esters and phenols were the major VFCs of soy sauce. The most important groups of volatile compounds in the soy sauce sample were ethanol, hexadecanoic acid, phenylethyl alcohol and 2,3-butanediol. In addition, some oxo-compounds and heterocyclic compounds were also found. The average relative standard deviation of the relative peak area was 12.1%, and the recoveries were 79.9%-109.6%. The method is simple, fast and accurate with high reproducibility, high sensitivity and low cost.

Key words: gas chromatography-mass spectrometry (GC-MS), soy sauce , volatile flavor compounds (VFCs), head space solid-phase microextractions (HS-SPME)