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Gdańsk University of Technology

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An in situ derivatization – dispersive liquid–liquid microextraction combined with gas-chromatography – mass spectrometry for determining biogenic amines in home-made fermented alcoholic drinks

A novel dispersive liquid–liquid microextraction (DLLME) gas chromatography mass-spectrometry(GC–MS) method was developed for the determination of 13 biogenic amines in home-made wine sam-ples. The method allows to simultaneous extraction and derivatization of the amines providing a simpleand fast mode of extract enrichment. During the study, two different procedures were examined. Sta-tistical analysis was performed to choose better procedure, as well as the conditions of derivatizationreaction. At least, a mixture of methanol (dispersive solvent; 215 L), chloroform (extractive solvent;400 L), and isobutyl choloroformate (derivatizing reagent; 90 L) was used as extractive/derivatizingreagent, added to 5 mL of sample. The addition of mixture of pyridine and HCl was necessary to elim-inate the by-products. The proposed method showed good linearity (correlation coefficients >0.9961),good recoveries (from 77 to 105%), and good intra-day precision (below 13%) and inter-day precision(below 10%). Moreover, detection limits were never over 4.1 g/L. The developed method was success-fully applied to the analysis of 17 home-made wine samples not regulated by law. All of the biogenicamines analyzed were found in most of the wines.

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