色谱

色谱 ›› 2017, Vol. 35 ›› Issue (2): 211-215.DOI: 10.3724/SP.J.1123.2016.09029

• 研究论文 • 上一篇    下一篇

热解产物逸出行为研究中新型内标释放装置的建立及其应用

朱文辉1, 杨柳2, 陈永宽2, 杨继2, 刘汗青3, 缪明明2   

  1. 1. 海南红塔卷烟有限责任公司, 海南 海口 571137;
    2. 云南中烟工业有限责任公司, 云南 昆明 650106;
    3. 瑞丽出入境检验检疫局, 云南 瑞丽 678600
  • 收稿日期:2016-09-12 出版日期:2017-02-08 发布日期:2013-06-09
  • 通讯作者: 朱文辉,Tel:(0898)65918853,E-mail:wh179@163.com
  • 基金资助:

    中国烟草总公司科技重大专项（110201401017（XX-05））.

Establishment of device used to release internal standard and its application to analysis of evolved behavior of pyrolysis products

ZHU Wenhui1, YANG Liu2, CHEN Yongkuan2, YANG Ji2, LIU Hanqing3, MIAO Mingming2   

  1. 1. Hainan Hongta Cigarette Co., Ltd., Haikou 571137, China;
    2. China Tobacco Yunnan Industrial Co., Ltd., Kunming 650106, China;
    3. Ruili Entry-Exit Inspection and Quarantine Bureau, Ruili 678600, China
  • Received:2016-09-12 Online:2017-02-08 Published:2013-06-09
  • Supported by:

    China National Tobacco Corporation of Science and Technology Major Project (No. 110201401017 (XX-05)).

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摘要：

实验在流动载气-液滴微萃取（GF-LDME）技术的基础上增加了液滴托附装置，设计并建立了内标物释放和热解产物富集的新型联用装置，使内标物和热解产物在相同条件下完成液滴的萃取和富集，实现了各温度段间目标热解产物相对含量的纵向比较。实验利用热重模拟咖啡生豆的烘焙过程，同时利用联用装置结合气相色谱-质谱研究了咖啡生豆在热重程序升温过程中发生的热解反应及其热解产物的逸出行为。热重条件：初始温度为50℃；以10℃/min升温至500℃；空气为载气。结果表明，在100~400℃范围内共发现13个热解产物，在280~300℃温度段，逸出量达到峰值的热解产物包括羟基丙酮、吡啶、糠醇、γ-丁内酯和正戊醛；在300~320℃温度段，逸出量达到峰值的热解产物包括乙酸、苯酚、2-环戊烯酮和愈创木酚。建立的联用装置在热解产物的逸出行为研究中具有明显优势。

关键词: 咖啡生豆, 流动载气-液滴微萃取, 内标释放装置, 热解, 热重, 逸出行为分析

Abstract:

Internal standard was applied to the analysis of evolved behavior of pyrolysis products. Liquid drop supporting device of gas flow-liquid drop microextraction (GF-LDME) was improved. The coupling device used to release internal standard and enrich the pyrolysis products was established. The internal standard and pyrolysis products were extracted into liquid drop under the same conditions. Coupled the device with gas chromatography-mass spectrometer (GC-MS), the comparison of relative amount for each pyrolysis product between different temperature ranges was achieved. The evolved behavior of pyrolysis products for green coffee beans was investigated. The experiments were conducted at a flowing air rate of 200 mL/min and a heating rate of 10℃/min. Identification of 13 pyrolysis products between 100℃ and 400℃ and the monitoring of evolved behavior were carried out. The hydroxyacetone, azabenzene, furfuryl alcohol, γ-butyrolactone and n-valeraldehyde evolved reached to a maximum evolved quantity at 280-300℃, while acetic acid, phenol, 2-cyclopentenone, 2-methoxyphenol evolved reached to a maximum quantity at 300-320℃. The method has obvious advantages in the analysis of complex pyrolysis products.

Key words: analysis of evolved behavior, gas flow-liquid drop microextraction (GF-LDME), green coffee beans, internal standard release device, pyrolysis, thermogravimetry (TG)

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