Development of HPLC method for quantitative determination of epimidin - new perspective АPhI with anticonvulsive activity

Authors

DOI:

https://doi.org/10.15587/2519-4852.2020.203181

Keywords:

Epimidin, pyrazolopyrimidine, anticonvulsant, quantitative determination, HPLC

Abstract

The aim. Development of optimal, high-precision and reproducible methods for quantitative determination of the main substance in the substance Epimidin - 1-(4-methoxyphenyl)-5-[2-[4-(4-methoxyphenyl)piperazin-1-yl]-2-oxo-ethyl]pyrazolo[3,4-d]pyrimidin-4-one by high performance liquid chromatography.

Materials and methods. High performance liquid chromatography (HPLC) was performed using a ShimadzuNexeraX2 LC-30AD system (Shimadzu, Japan) equipped with a SPD-M20A diode array detector (DAD). ACE C18 column, size 250 x 4.6 mm, YMC with pre-column, particle size 5 μm, filled with octylsilyl silica gel for chromatography P. During the work acetonitrile and trifluoroacetic acid of HPLC class (Sigma-AldrichGmbH, Switzerland) were used, other chemicals and solvents were of analytical grade. In the study an analytical ware class A were used that meet the requirements of SPhU.

Results. The following optimal conditions of chromatographic distribution are established: column C18 (250*4.6 mm); the speed of the mobile phase 1 ml / min; column thermostat temperature 35 °С; injection volume 10 μl; mobile phase A - 0.1 % trifluoroacetic acid; mobile phase B - acetonitrile P; the detection wavelength is 270 nm, the retention time of the test compound is 7.22 minutes. The performance of the column was determined for its main indicators, such as the number of theoretical plates (more than 25410) and the coefficient of symmetry (about 1.00). The technique was tested for the influence of various factors, such as flow rate, mobile phase composition and column thermostat temperature. It was established that the influence of these factors is insignificant and does not affect the results obtained by this method. The method was validated in accordance with the recommendations of SPhU on the parameters of specificity, linearity, correctness, precision, robustness (stability).

Conclusions. For the first time, a high-precision and reproducible method for quantitative determination of the main substance in the substance Epimidin with anticonvulsant activity by high-performance liquid chromatography was developed. Conditions for chromatographic analysis (HPLC) were standardized. The requirements for the test “System suitability test criteria for chromatographic methods” are set. Statistical processing of the experimental results shows that the relative uncertainty of the average result is within acceptable limits. The correctness of the method was confirmed by validation studies. The developed technique will be used for pharmaceutical development and standardization of dosage form

Author Biographies

Hanna Severina, National University of Pharmacy Pushkinska str., 53, Kharkiv, Ukraine, 61002

PhD, Associate Professor

Department of Pharmaceutical Chemistry

Ivan Bezruk, National University of Pharmacy Pushkinska str., 53, Kharkiv, Ukraine, 61002

Postgtaduate Student

Department of Pharmaceutical Chemistry

Liudas Ivanauskas, Lithuanian University of Health Sciences Mickevičiaus g. 9, Kaunas, Lithuania, LT 44307

Doctor of Biomedical Sciences, Professor, Head of Department

Department of Analytical and Toxicological Chemistry

Victoriya Georgiyants, National University of Pharmacy Pushkinska str., 53, Kharkiv, Ukraine, 61002

Doctor of Pharmaceutical Sciences, Professor, Head of Department

Department of Pharmaceutical Chemistry

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Published

2020-06-30

How to Cite

Severina, H., Bezruk, I., Ivanauskas, L., & Georgiyants, V. (2020). Development of HPLC method for quantitative determination of epimidin - new perspective АPhI with anticonvulsive activity. ScienceRise: Pharmaceutical Science, (3 (25), 4–11. https://doi.org/10.15587/2519-4852.2020.203181

Issue

No. 3 (25) (2020)

Section

Pharmaceutical Science

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