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.

Preparation of arginine-modified reduced graphene oxide composite filled in an on-line solid-phase extraction disk and its application in the analysis of heterocyclic aromatic amines

“…Sample preparation techniques are developed for decreasing organic solvent consuming, increasing enrichment of target compounds and purifying the sample. Combined with different sample preparation techniques, different analytical techniques, such as CE, HPLC combined with UV–Vis diode array (DAD), fluorescence or MS, GC–MS and UHPLC–ESI‐MS/MS have been applied to the detection of HAAs in different matrices . Compared with the GC–MS method, HAAs are directly detected by HPLC without an additive derivatization step for target compounds .…”