mass-spectrometry-congress-2019-posters-abstracts

Page 54

May 20-21, 2019 | Rome, Italy

OF EXCELLENCE

IN INTERNATIONAL

MEETINGS

YEARS

Journal of Chemical Technology and Applications | Volume 3

MASS SPECTROMETRY,

PROTEOMICS AND POLYMER CHEMISTRY

International Conference on

Mass Spectrometry Congress 2019

PECULIARITIES OF GAS CHROMATOGRAPHIC MASS SPECTROMETRIC DETERMINATION

OF O-PHTHALIC ACID ESTERS IN ALCOHOLIC BEVERAGES AND ETHANOL COUPLED

WITH EMULSION LIQUID-PHASE MICROEXTRACTION PRE-CONCENTRATION

Krylov V

Nizhny Novgorod State University, Russia

ialkyl o-phthalates are very dangerous compounds. In this study the high sensitive gas chromatograph-

ic-mass spectrometric determination of phthalates in wines (sparkling, red and white wine), strong alco-

holic beverages and ethanol coupled ultrasound-assisted emulsification-microextraction was developed. In

the case of pre-concentration of impurities from alcohol dilution was carried out with purified water. N-Octane,

n-hexane and m-xylene were used as extractants. De-emulsification of extracts was carried out by centrifuga-

tion and flotation. The sources of possible systematic errors were investigated: leaking of o-phthalates from

chromatographic septum; contamination of phthalates in solvents; influence of macro components of wines

(sugar, alcohol and anthocyanin’s); 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 pro-

posed. Purification of solvents by Rayleigh distillation method allows obtaining samples with impurity content

lower than (1-4)10-3 mgL-1. Containers for sampling and storage of samples to be analyzed should be made

of borosilicate glass or quartz. The limits of detection of esters of о-phthalic acid are at the level of 10-6–10-5

mgL-1 and are highly competitive with the best world results. The content of o-phthalates in wines and strong

alcoholic beverages was 0.03-1, in ethanol –0.01-30 mgL-1. The relative expanded uncertainty of the determi-

nation of toxicants is at the level of 13-30%.

J Chem Tech App 2019, Volume 3