VALIDATION OF THE ANALYTICAL PROCEDURE FOR ENISAMIUM IODIDE QUANTITATIVE DETERMINATION IN ACTIVE PHARMACEUTICAL INGREDIENT BY THE HIGH PERFOMANCE LIQUID CHROMATOGRAPHY METHOD
DOI:
https://doi.org/10.11603/2312-0967.2019.1.9952Keywords:
enisamium iodide, active pharmaceutical ingredient, assay, high performance liquid chromatography, validationAbstract
The aim of the work. The work is devoted to development and validation of the analytical procedure for enisamium iodide quantitative determination in active pharmaceutical ingredient by the high performance liquid chromatography method.
Materials and Methods. The reference standard of enisamium iodide and the sample of active pharmaceutical ingredient produced by Farmak JSC were used. During the work, an optimal sample injection volume of 10 μl, a detection wavelength of 225 nm, chromatographic conditions and requirements for the suitability of the chromatographic system were established. The study was carried out using Agilent 1200 liquid chromatograph equipped with a degasser, a four-channel pump, automatic sampler, a chromatographic column thermostat and a diode array detector. The Zorbax Eclipse XDB-C18 chromatographic column, 150 x 4.6 mm size, filled with octadecylsilyl sorbent, with a particle size of 5 μm, was used.
Results and Discussion. The selectivity of the analytical method was confirmed.
Validation of the analytical procedure was carried out in accordance with the recommendations of the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) [1].
Linearity studies were performed on model solutions in which the concentration of enisamium iodide varied linearly in the range from 80 % to 120 % relative to the nominal concentration (0.4 mg/ml) of enisamium iodide in the test solution.
Validation characteristics such as specificity, accuracy, precision, and robustness were confirmed.
The correlation coefficient (r) between the the fitted and observed values (r) for enisamium iodide was 0.99995.
Conclusions. It was experimentally established that the described analytical procedure can be used for enisamium iodide assay test of active pharmaceutical ingredient.
References
Boltz D, Peng X, Muzzio M, Dash P, Thomas P, Mehta R, et al. Antiviral activity of enisamium against influenza viruses in differentiated normal human bronchial epithelial cells. Proceedings of the 3rd Antivirals Congress; 2014 Oct 12-14; Amsterdam, Netherlands.
Bolts D, Pen S, Muzzio M, Dash P, Tomas P, Mekhta R, et al. Antiviral activity of enisamium (Amizon) against influenza viruses in differentiated normal human bronchial epithelial cells. [Противовирусная активность энисамиума (Амизона) в отношении вирусов гриппа в дифференцированных нормальных клетках эпителия бронхов человека]. Russkiy meditsinskiy zhurnal. 2015;2:72-4. Russian.
International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (Chemical Substances Q6A). (1999). Specifications: Test Procedures and Acceptance Criteria for New Drug Substance and New Drug Products
European Medicines Agency (Guideline Q2 (R1)). (1995). Validation of analytical procedures: text and methodology.
Burmaka АV, Hureyeva SN, Marhitich VM. (2017). Razrabotka metodiki kontrolya soputstvuyushchikh primesey substantsii enisamiuma yodida [Development of HPLC method for the determination of related substances in API enisamium iodide]. Farmakom, 3, 17-25. Russian.
Burmaka OV, Hureyeva, SM, Marhitich VM. (2018). Validatsiia metodyky vyznachennya suprovidnykh domishok v aktyvnii rechovyni enisamiumu iodydu [Validation of the method for determination of related substances in active antiviral ingredient of enisamium iodide]. Zaporozhskiy meditsinskiy zhurnal – Zaporozhye Medical Journal, 5, 708-716. Ukrainian.
Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines. State Pharmacopoeia of Ukraine. [Державна Фармакопея України]. 2nd ed. Vol. 1. Kharkiv: Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines; 2015. Ukrainian.
Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines. State Pharmacopoeia of Ukraine. [Державна Фармакопея України]. 2nd ed. Vol. 1. Kharkiv: Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines; 2015. Ukrainian.
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