色谱

色谱 ›› 2013, Vol. 31 ›› Issue (1): 4-9.DOI: 10.3724/SP.J.1123.2012.09011

• 研究快报 • 上一篇    下一篇

耐压多样品微量衍生反应装置在气相色谱-质谱联用法分析极性杂环胺中的应用

王翊如1, 陈方翔1, 施雅梅2, TAN Connieal1, 陈曦1*   

  1. 1. 厦门大学化学化工学院化学系 分析科学重点实验室, 福建 厦门 361005; 2. 厦门出入境检验检疫局检验检疫技术中心, 福建 厦门 361012
  • 收稿日期:2012-09-07 修回日期:2012-11-09 出版日期:2013-01-28 发布日期:2013-01-21
  • 通讯作者: Tel: (0592)2184530.
  • 基金资助:

    国家自然科学基金项目(21105084)；福建省自然科学基金项目(2009J01042)；福建省科技重大专项专题项目（2011YZ0001-1）.

Applications of multi-micro-volume pressure-assisted derivatization reaction device for analysis of polar heterocyclic aromatic amines by gas chromatography-mass spectrometry

WANG Yiru1, CHEN Fangxiang1, SHI Yamei2, TAN Connieal1, CHEN Xi1*   

  1. 1. Department of Chemistry & Key Laboratory of Analytical Science, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China; 2. Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China
  • Received:2012-09-07 Revised:2012-11-09 Online:2013-01-28 Published:2013-01-21
  • Contact: Xi

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摘要： 设计并制作了耐压多样品微量衍生反应装置。在该装置中采用N-(叔丁基二甲基硅烷基)-N-甲基三氟乙酰胺(MTBSTFA,含1%叔丁基二甲基氯硅烷)硅烷化试剂高温衍生极性杂环胺,衍生产物可以直接在气相色谱-质谱联用仪上分析。使用该装置,既可以在比试剂沸点高的温度下实现衍生反应,也可以实现多个微量样品的同时衍生。着重考察了衍生化过程中反应瓶的顶空体积、试剂蒸发面积、温度、时间等实验条件的影响。结果表明,在90 ℃衍生时,与普通衍生装置相比,使用耐压衍生装置可以有效地减小挥发损失,显著增大衍生产量;在150 ℃衍生时,由于试剂挥发损失严重导致普通衍生装置无法使用,而采用耐压衍生装置却可以实现定量衍生,但通过加温加压方式来加快衍生反应速率的效果并不十分明显。

关键词: 极性杂环胺, 耐压装置, 气相色谱-质谱法, 衍生

Abstract: A multi-micro-volume pressure-assisted derivatization reaction device has been designed and made for the silylation derivatization of polar heterocyclic aromatic amines by N-(tert-butyldimethylsilyl)-N-methyl-trifluoroacetamide (MTBSTFA) with 1% catalyst tert-butyldimethylchlorosilane (TBDMCS) at a high temperature. The tert-butyldimethylsilyl derivatives then could be automatically analyzed by gas chromatography-mass spectrometry. Using the pressure-assisted device, the silylation reaction may occur at a temperature higher than the boiling points of the reagents, and several micro-volume samples can be simultaneously pretreated in the same device to shorten the sample-preparation time and to improve the repeatability. The derivatization conditions including the headspace volume of the vial, the evaporative surface area of the reagent, derivatization temperature and time have been discussed for the use of the pressure-assisted device. The experimental results proved that the device is an effective way for the simultaneous derivatization of several micro-volume samples at a high temperature. Compared with a common device, the derivative amounts were obviously increased when using the pressure-assisted device at 90 ℃. Quantitative derivatization can be achieved even at 150 ℃ while there was no common device could be applied at such a high temperature due to the heavy losses of reagents by evaporation. However, no obviously higher reaction speed has been observed in such a circumstance with a higher temperature and a higher pressure using the pressure-assisted device.

Key words: gas chromatography-mass spectrometry (GC-MS), polar heterocyclic aromatic amines, pressure-assisted device, derivatization