色谱

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冷柱头程序升温进样-气相色谱/质谱法研究新鲜大蒜中的有机硫化合物

郑屏1,盛旋1,丁袁生1,胡艳云2

  

  1. 1.Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230061, China;
    2.Department of Chemistry, University of Science and Technology of China, Hefei 230026, China

  • 收稿日期:2005-08-18 修回日期:2005-10-27 出版日期:2006-07-30 发布日期:1986-12-25
  • 通讯作者: 郑屏

Study of Organosulfur Compounds in Fresh Garlic by Gas Chromatography/Mass Spectrometry Incorporated
with Temperature-Programmable Cold On-Column Injection

ZHENG Ping1, SHENG Xuan1, DING Yuansheng1, HU Yanyun2

  

  1. 1.Anhui Entry-Exit Inspection and Quarantine Bureau, Hefei 230061, China;
    2.Department of Chemistry, University of Science and Technology of China, Hefei 230026, China

  • Received:2005-08-18 Revised:2005-10-27 Online:2006-07-30 Published:1986-12-25
  • Contact: Zheng Ping

摘要:

采用冷溶剂提取新鲜大蒜中的有机硫化合物,结合冷柱头程序升温进样,对大蒜原始组分进行了气相色谱/质谱分析
。该法实现了从提取到色谱分离的“冷过程”,因而可以准确地鉴定大蒜提取液在热分解前的原始组分。分析结果表明,
在大蒜提取液中含有3-乙烯基-1,2-二硫杂-5-环己烯及其异构体2-乙烯基-1,3-二硫杂-4-环己烯两种主要组分以及少量
的S-甲基甲烷硫代亚磺酸酯、二烯丙基二硫醚、二烯丙基三硫醚。对大蒜的冷溶剂提取液和水蒸气蒸馏提取的大蒜油中
的有机硫化合物进行了比较,对一些主要有机硫化合物的形成进行了初步探讨。

关键词: 程序升温进样, 大蒜 , 冷柱头, 气相色谱/质谱法, 有机硫化合物

Abstract:

For the analysis of organosulfur compounds in fresh garlic, a gas chromatographic/mass
spectrometric (GC/MS) method is proposed using temperature-programmable cold on-column injection
and cold solvent extraction of the fresh garlic. This was carried out under the conditions of
cryogenic process from extraction to column separation. Hence, a valid identification can be
achieved about the primary components in garlic extract before thermo-degradation. The obtained
results showed that 3-vinyl-4H-1,2-dithiin and 2-vinyl-4H-1,3-dithiin were the major compounds in
the garlic extract with minor amounts of S-methyl methanethiosulfinate, diallyl disulfide,
trisulfide-di-2-propenyl. A comparative study of chemical compounds was performed between garlic
extract by cold solvent and garlic oil by stream distillation. The degradation and formation of
major organosulfur compounds in the garlic extract were also explored.

Key words: cold on-column, garlic , organosulfur compounds, temperature-programmable
inlet,
gas chromatography/mass spectrometry (GC/MS)