euro-gastroenterology-clinical-pharmacy-2019-accepted

Euro Gastroenterology 2019 & Clinical Pharmacy 2019

Archives of General Internal Medicine | ISSN: 2591-7951 | Volume 3

Page 56

Note:

March 25-26, 2019 | Amsterdam, Netherlands

GASTROENTEROLOGY AND HEPATOLOGY

International Conference on

CLINICAL PHARMACY & PHARMACY PRACTICE

World Congress on

Joint Event on

OF EXCELLENCE

IN INTERNATIONAL

MEETINGS

YEARS

GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC DETERMINATION

OF ESTERS OF O-PHTHALIC ACID IN PHARMACEUTICAL ETHANOL

COUPLEDWITH EMULSION LIQUID-PHASE MICROEXTRACTION

PRECONCENTRATION

Krylov V, Mosyagin P

and

Mysyagina E

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 ethanol coupled ultrasound-assisted emulsifica-

tion-microextraction was developed. In the case of preconcentration of impurities from ethanol 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 centrifugation and flotation.The sources of possible systematic errors were in-

vestigated: leaking of o-phthalates from chromatographic septum; contamination of phthalates in solvents;

influence of ethanol; 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. Purifi-

cation of solvents by Rayleigh distillation method allows to obtain 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 borosili-

cate 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 ethanol was 0.01-30 mgL-1.

The relative expanded uncertainty of the determination of toxicants is at the level of 13- 30%.

Arch Gen Intern Med 2019, Volume 3 | DOI: 10.4066/2591-7951-C1-024