title: An in situ derivatization - dispersive liquid-liquid microextraction combined with gas-chromatography - mass spectrometry for determining biogenic amines in home-made fermented alcoholic drinks.
abstract: 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 samples. The method allows to simultaneous extraction and derivatization of the amines providing a simple and fast mode of extract enrichment. During the study, two different procedures were examined. Statistical analysis was performed to choose better procedure, as well as the conditions of derivatization reaction. At least, a mixture of methanol (dispersive solvent; 215μL), chloroform (extractive solvent; 400μL), and isobutyl choloroformate (derivatizing reagent; 90μL) was used as extractive/derivatizing reagent, added to 5mL of sample. The addition of mixture of pyridine and HCl was necessary to eliminate 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 4.1μg/L. The developed method was successfully applied to the analysis of 17 home-made wine samples not regulated by law. All of the biogenic amines analyzed were found in most of the wines.
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology, 11/12 Narutowicza Street, 80-233 Gdańsk, Poland. Electronic address: plotkajustyna@gmail.com.
authors.forename: Justyna
authors.initials: J
authors.lastname: Płotka-Wasylka
authors.affiliation: Faculty of Chemistry and Pharmacy, University of Sofia, 1 James Bourchier Blvd., Sofia 1126, Bulgaria.
authors.forename: Vasil
authors.initials: V
authors.lastname: Simeonov
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology, 11/12 Narutowicza Street, 80-233 Gdańsk, Poland.
authors.forename: Jacek
authors.initials: J
authors.lastname: Namieśnik
mesh_terms: D001679:Biogenic Amines / Q000032:analysis* / Q000302:isolation & purification; D002725:Chloroform; D005285:Fermentation; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D000432:Methanol; D012997:Solvents / Q000032:analysis; D014920:Wine / Q000032:analysis*
chemical_list: D001679:Biogenic Amines; D012997:Solvents; D002725:Chloroform; D000432:Methanol
keywords: Biogenic amines; DLLME; Derivatization; Experimental design; GC–MS