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  

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

作　　者：王翊如[1] 陈方翔[1] 施雅梅[2] TAN Connieal 陈曦[1] 

机构地区：[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

出　　处：《色谱》2013年第1期4-9,共6页Chinese Journal of Chromatography

基　　金：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)

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。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 deriva- tives 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 pre- treated in the same device to shorten the sample-preparation time and to improve the repeat- ability. The derivatization conditions including the headspace volume of the vial, the evapora- tive 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 tem- perature. 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 pres- sure using the pressure-assisted device.

关 键 词：衍生 耐压装置 气相色谱-质谱法 极性杂环胺 

分 类 号：O658[理学—分析化学]