Validation of a simple reversed Phase-HPLC method for determination of Blacofen in tablets
DOI:
https://doi.org/10.22456/2527-2616.87929Keywords:
Baclofen, baclofen tablets, validation, stability indicativeAbstract
Baclofen is a muscle relaxant used as a first option to treat spasticity and muscle spasms in patients with spinal cord injuries, which is available in Brazil as 10 mg tablets. The compendia methods employ HPLC by ion pairing that requires the use of specific reagents and column conditioning, increasing the waste generation and the cost of analysis. In this study, an isocratic, simple and stability-indicating HPLC method was validated to assay baclofen tablets. A C-18 column (Luna®, 150 x 4.6 mm, 5μm), mobile phase composed by triethylamine 10 mM pH 7.0, methanol and acetonitrile (80:15:5), flow rate 1 mL/min and detection at 220 nm was used. The baclofen retention time was 6.2 min and the method was linear in the range of 5 – 100 μg.mL-1 (r = 0.9999). Method selectivity was demonstrated by the forced degradation study and simultaneous analysis of baclofen impurity. The method showed accuracy (mean recovery 99.27%) and precision (RSD < 2%). The robustness was evaluated by factorial design, and the method was robust robust regarding the proposed variations. The developed method met the requirement of current guidelines, being indicative of stability and suitable for the determination of baclofen in tablets.
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Quagliato E, Bang G, Botelho LA, Gianini MAC, Spósito MMM, Lianza S. Espasticidade: Tratamento Medicamentoso. Available from: URL: http://www.projetodiretrizes.org.br/5_volume/21-
Pereira CU, Santos CMT, Santos EGS. Tratamento medicamentoso da espasticidade. J. Bras. Neurocirurg. 2003; 14(2): 55-59.
Brunton L, Parker KL, Blumenthal DK, Buxton ILO. Goodman & Gilman: Manual de Farmacologia e Terapêutica: O Manual Portável do Melhor LivroTexto de Farmacologia do Mundo. AMGH, 2014.
USP 38.The United States Pharmacopeia. 38ed. Rockville: United States Pharmacopeial Convention, 2015.
BP 2013. British Pharmacopoeia. London: The Stationary Office, 2013.
Collins H. Introdução a métodos cromatográficos; 7th ed. Editora da Unicamp, Campinas; 1997.
Watson GD. Pharmaceutical Analysis: A textbook for pharmacy students and pharmaceutical chemists, 2nd ed. Churchill Livingstone: London; 2005.
Dukova AO, Krasnov EA, Efremov AA. Development of an HPLC method for determining baclofen. Pharm. Chem. J. 2015; 48(10): 687-689.
Raul SK, Ravi Kumar BVV, Pattnaik AK, Sahoo PK. RP-HPLC Method development and validation for the estimation of baclofen in bulk and pharmaceutical dosage forms. Int. J. Chem. Sci. 2013; 11 (1): 390- 398.
Cao LW, Li C. Rapid and sensitive analysis of baclofen by high-performance liquid chromatography with UV-vis and FD detection. Acta Chromatogr. 2012; 24(3): 383-397.
Nalluri BN, Sushmitha B, Sunandana B, Prasad-Babu D. Development and validation of RP-HPLC-PDA method for simultaneous estimation of baclofen and tizanidine in bulk and dosage forms. J. Appl. Pharm. Sci. 2012; 2 (7): 111-116.
Hanafi R, Mosad S, Abouzid K, Nieb R, SpahnLangguth, H. Baclofen ester and carbamate prodrug candidates: A simultaneous chromatographic assay, resolution optimized with DryLab® . J. Pharm. Biomed. Anal. 2011; 56: 569-576.
Rustum AM. Simple and rapid reversed-phase highperformance liquid chromatographic determination of baclofen in human plasma with ultravioleta detection. J. Chromatogr. 1989; 487: 107-105. 14. Millerioux L, Brault M, Gualano V, Mignot A. Highperformance liquid chromatographic determination of baclofen in human plasma. J. Chromatogr. A. 1996; 729: 309-314.
Hefnawy MM, Aboul-Enein HY. Enantioselective high-performance liquid chromatographic method for the determination of baclofen in human plasma. Talanta. 2003; 61: 667-673.
Zhu Z, Neirinck L. Chiral separation and determination of R-(-)- and S-(+)-baclofen in human plasma by high-performance liquid chromatography. J. Chromatogr. B. 2003; 785: 277–283. 17. Silva KER, Alves LDS, Soares MFR, Passos RCS, Faria AR, Rolim Neto PJ. Modelos de avaliação da estabilidade de fármacos e medicamentos para a indústria farmacêutica. Rev. Cienc. Farm. Basica Apl. 2009; 30 (2): 129-135.
TØnnesen HH. Formulation and stability testing of photolabile drugs. Int. J. Pharm. 2001; 225: 1-14.
Bakshi M, Singh S. Development of validated stability-indicating assay methods – critical review. J. Pharm. Biomed. Anal. 2002; 28: 1011 -1040.
Taborianski AM. Validação de métodos analíticos para análise e estudos de estabilidade de anti-retrovirais em preparações farmacêuticas. São Paulo. Dissertação [Mestrado em Fármacos e Medicamentos], Universidade de São Paulo; 2003.
Vehabovic M, Hadzovic S, Stambolic F, Hadzic A, Vranjes E, Haracic E. Stability of ranitidine in injectable solution. Int. J. Pharm. 2003; 256: 109-115.
Brazil. Agência Nacional de Vigilância Sanitária. 2017. Resolução RDC n° 166 de 27 de julho de 2017. Dispõe sobre a validação de métodos analíticos e dá outras providências, Diário Oficial da União: Brasília.
Baclofen monography. Available from: https://www.drugbank.ca/unearth/q?utf8=%E2%9C %93&query=baclofen&searcher=drugs.
Brasil. Agência Nacional de Vigilância Sanitária. 2015. Resolução RDC n° 53 de 04 de dezembro de 2015. Estabelece parâmetros para a notificação, identificação e qualificação de produtos de degradação em medicamentos com substâncias ativas sintéticas e semissintéticas, classificados como novos, genéricos e similares, e dá outras providências. Diário Oficial da União: Brasília.
Alsante MK, Ando A, Brown R, Ensing J, Hatajik TD, Kong W, et al. The role of degradant profiling in active pharmaceutical ingredients and drug products. Adv Drug Deliv Rev. 2007; 59: 29-37.
Shabir GA. Validation of high-performance liquid chromatography methods for pharmaceutical analysis Understanding the differences and similarities between validation requirements of the US Food and Drug Administration, the US Pharmacopeia and the International Conference on Harmonization. J. Chromatogr. A. 2003; 897: 57-66.
International Conference on Harmonization (ICH), Validation of Analytical Procedures: Text and Methodology, Q2 (R1), 2005.
Dejaegher B, Heyden YV. Ruggedness and robustness testing. J. Chromatogr. A. 2007; 1158: 138–157.
Neto BB, Scarminio IS, Bruns RE. Como fazer experimentos – pesquisa e desenvolvimento na ciência e na indústria, Ed Unicamp: Campinas:2001.
Lenth RV. Quick and easy analysis of unreplicated factorials. Technometrics; 1989; 31 (4): 469–473.
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