DEVELOPMENT AND VALIDATION OF THE METHOD OF QUANTITATIVE DETERMINATION OF FLUORINE-CONTAINING DRUGS BY THE METHOD OF HIGHLY EFFECTIVE LIQUID CHROMATOGRAPHY

DOI: https://doi.org/10.29296/25877313-2019-12-04
Issue: 
12
Year: 
2019

V.A. Tyutrina Post-graduate Student, Department of Pharmaceutical and Toxicological Chemistry, Irkutsk State Medical University E-mail: ultr4vox@yandex.ru N.V. Chmelevskaya Ph.D. (Pharm.), Head of Head of the Department of Forensic Chemistry, Irkutsk Regional Bureau of Forensic Medicine E.A. Illarionova Dr.Sc. (Chem.), Professor, Head of Department of Pharmaceutical and Toxicological Chemistry, Irkutsk State Medical University

Objective. To develop and validate methods for the quantitative determination of fluorine-containing drugs in tablets by high performance liquid chro-matography. Material and methods. In the work we used: pharmaceutical substance and tablets of linezolid, efavirenza and ofloxacin, which meet the requirements of regulatory documents. To develop methods for detecting and quantifying linezolid, efavirenz, and ofloxacin in tablets, a reverse-phase version of high-performance liquid chromatography in gradient elution was used, the conditions of which were selected experimentally. Optimal chromatographic conditions: column size - 75 × 2 mm, polymer sorbent - ProntoSil 120-5C AQ, mobile phase - Eluent A: 0.2 M LiClO4 - 0.005 M HClO4 (pH 2,8), Eluent B: Acetonitrile, gradient: 3700 μl from 5% to 70% eluent B, flow rate 100 μl / min, column temperature 40 ° C, sample volume 2 μl, wavelength 210 nm. Results. The conditions found were used to develop methods for the quantitative content of these substances in tablets. The retention times of oflox-acin were 15.39 minutes, linezolid 16.16 minutes and efavirenza 34.49 minutes. The relative error of the quantitative determination by the developed methods does not exceed 1.22% for ofloxacin, 1.08% for linezolid and 1.39% for efavirenz. Findings. During the study, unified methods were devel-oped for the quantitative determination of fluorine-containing heterocyclic drugs - linezolid, efavirenz, and ofloxacin in tablets by high-performance liquid chromatography. A validation assessment of the developed methods was carried out. Thus, the developed methods make it possible to obtain suffi-ciently reliable and reproducible results for the intended field of application and can be recommended for pharmaceutical, chemical-toxicological, and forensic chemical analysis.

Keywords: 
ofloxacin
linezolid
efavirenz
high performance liquid chromatography
quantitation

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