V.A. Krylov
N. I. Lobachevskii Nizhny Novgorod State University, Russia
Title: Features of Gas Chromatography-Mass Spectrometry Determination of o-Phthalates in Low Alcohol Wines with Liquid-Liquid Microextraction
Biography
Biography: V.A. Krylov
Abstract
Esters of phthalic acid are very dangerous for human health. Their penetration into the organism leads to the occurrence of cancer, disease of liver, kidney, reproductive organs. Phthalates are very widespread toxicants. Their occurrence in wines is connected with the inflow from the plasticized polymer seals, plastic piping, tanks and stoppers. In this study the high sensitive gas chromatographic-mass spectrometric determination of phthalates in low alcoholic beverages (champagne, red and white wine) coupled ultrasound-assisted emulsification-microextraction was developed. As extractants environmentally friendly hydrocarbons - octane and n-hexane are proposed. The sources of possible systematic errors were investigated: leaking of o-phthalates from chromatographic septum; contamination of phthalate in solvents; influence of macro components of wines; the hydrolysis of o-phthalates and others. For the first time it is shown that the impact of these factors can lead to an overestimation or underestimation of the actual concentration of impurities by 1-2 orders of magnitude. The methods of accounting or elimination of systematic errors are proposed. The content of phthalates in wines was 0.03 - 1 mgL-1. The largest concentrations are characteristic for diethyl-, di-n-butyl- and di(2-ethylhexyl) phthalates. The limits of detection of esters of о-phthalic acid in low alcohol beverages achieved are at the level of 10-6–10-5 mgL-1 and are highly competitive with the best world results. The relative expanded uncertainty of the determination of toxicants of 13- 30%.