title: [Applications of multi-micro-volume pressure-assisted derivatization reaction device for analysis of polar heterocyclic aromatic amines by gas chromatography-mass spectrometry].
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 degrees C. Quantitative derivatization can be achieved even at 150 degrees C 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.
authors.affiliation: Department of Chemistry & Key Laboratory of Analytical Science, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China.
authors.forename: Yiru
authors.initials: Y
authors.lastname: Wang
authors.forename: Fangxiang
authors.initials: F
authors.lastname: Chen
authors.forename: Yamei
authors.initials: Y
authors.lastname: Shi
authors.forename: Connieal
authors.initials: C
authors.lastname: Tan
authors.forename: Xi
authors.initials: X
authors.lastname: Chen
mesh_terms: D000588:Amines / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D006571:Heterocyclic Compounds / Q000032:analysis*
chemical_list: D000588:Amines; D006571:Heterocyclic Compounds