Development of single‐drop microextraction and simultaneous derivatization followed by GC‐MS for the determination of aliphatic amines in tobacco

Abstract

In this work, for the first time, headspace (HS) single-drop microextraction and simultaneous derivatization followed by GC-MS was developed to determine the aliphatic amines in tobacco samples. In the HS extraction procedure, the mixture of derivatization reagent and organic solvent was employed as the extraction solvent for HS single-drop microextraction and in situ derivatization of aliphatic amine in the samples. Fast extraction and simultaneous derivatization of the analytes were performed in a single step, and the obtained derivatives in the microdrop extraction solvent were analyzed by GC-MS. The optimized experiment conditions were: sample preparation temperature of 80 degrees C and time of 30 min, HS extraction solvent (the mixture of benzyl alcohol and 2,3,4,5,6-pentafluorobenzaldehyde) volume of 2.0 microL, extraction time of 90 s. With the optimal conditions, the method validations were also studied. The method has good linearity (R(2) more than 0.99), accepted precision (RSD less than 13%), good recovery (98-104%) and low limit of detection (0.11-0.97 microg/g). Finally, the proposed technique was successfully applied to the analyses of aliphatic amines in tobacco samples of seven different brands. It was further demonstrated that the proposed method offered a simple, low-cost and reliable approach to determine aliphatic amines in tobacco samples.

Chemical Derivatization Processes Applied to Amine Determination in Samples of Different Matrix Composition

“…In the last few years, many different derivatization methods of amine have been developed for SDME [109][110][111] . Previously, derivatization followed by SDME was the most commonly used for the analysis of amine compounds 130 .…”

A glance at achievements in the coupling of headspace and direct immersion single‐drop microextraction with chromatographic techniques

“…One can find, however, various modifications of SDME that more or less differ from the above‐described general procedure. Examples of the application the two most commonly used modes of SDME—HS and DI—can be found in the Supporting Information …”

Simultaneous determination of pesticide multiresidues in white wine and rosé wine by SDME/GC-MS

“…After the extraction, the microdrop is retracted into the microsyringe and injected into instruments for liquid or gas chromatography for analysis [8,10]. This technique has been successfully used in the determination of different classes of substances, such as phenolic compounds [11], sulfur compounds [12], metals [13,14] and amines [15], as well as for the extraction of pesticides [8,[16][17][18][19] in different matrices.…”