J Chromatogr Sci. 2015 Apr 23. pii: bmv044. [Epub ahead of print]
A new method for the determination of sucrose in honey with derivatization solid-phase microextraction and gas chromatography/mass spectrometry (D-SPME-GC/MS) was developed. The method incorporates a sample derivatization with acetic anhydride using N-methylimidazole as the catalyst and the subsequent enrichment of the analyte in a Polyacrylate-SPME fiber.
Results show that 100 µL N-methylimidazole and 800 µL acetic anhydride were sufficient to complete the acetylation for sucrose in 100 µL aqueous sample at room temperature. For SPME, an enrichment time of 30 min was sufficient. SPME was performed by immersing the fiber into the solution with additional vibration. Then, the analyte was desorbed for 5 min at 280°C in the GC/MS injection port with splitless mode. The present method exhibits good linearity at a concentration range of 0.3-8% of sucrose in honey with excellent regression (R = 0.9993). The method has been successfully applied to the control of sucrose adulteration in honey.