Simultaneous Extraction and Derivatization of Volatile Organic Acids in Flue-Cured Tobacco with Headspace Solid-Phase Microextraction Followed by GC-MS

Abstract

Simultaneous extraction and derivatization followed by head-space solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC-MS) was employed to determine volatile organic acids (VOAs) in flue-cured tobacco samples. Several experimental parameters, such as the type of SPME fibers, sampling temperature, pre-extraction and derivatization equilibration time, and anhydrous sodium sulfate amount, were optimized to improve sampling efficiency. Validation was carried out in terms of limits of detection (LOD), precision, recovery, and linearity. The results indicated that the optimized technique was easy, highly efficient, and sensitive. Finally, the performance of the proposed method was tested for the extraction and determination of the VOAs in flue-cured tobacco and satisfactory results were achieved.

Keywords:

• Derivatization
• Flue-cured tobacco
• GC-MS
• Head-space solid phase microextraction
• Volatile organic acids

Acknowledgments

This work was supported by the Science Foundation of Guizhou Tobacco Corporation of China (No. 201112 and No. 200920) for financial support.

Notes

^a RSD is relative standard deviation (n = 5).

^b LOD was obtained on the basis of three times standard deviation of five replicate tests at “zero-point,” that is not spiked.

^c A standard mixture solution of 5.0 μL was spiked into the flue-cured tobacco sample.

^a All flue-cured tobacco samples were from the 2010 crop year; Variety: K326; Grade: C3 F. All values are mean ±SD obtained by five analyses.