Method validation for the quantification of fluconazole and its organic impurities in raw material using high-performance liquid chromatography
Abstract
Introduction. The real laboratory conditions of each country, including climate, can affect the method’s efficiency in analyzing a pharmacological substance. Thus, it is necessary to validate the process according to the corresponding guidelines and optimize it to ensure success and confidence in the results.
Objective. The objective was to validate a methodology for fluconazole and its organic impurities quantification in raw material using high-performance liquid chromatography, with a diode array detector, under tropical climate conditions, and complying with all regulatory requirements.
Materials and methods. We performed pre-validation tests of the method consisting of system adequacy, filters study, quantification limit, absence of systematic error, forced degradation studies, and solutions stability. In addition, we validated the specificity, linearity, accuracy, precision, and robustness of the system.
Results. Separation of the degradation products from the analyte peaks allowed the achievement of the method’s spectral purity. The solution’s stability was not affected during the evaluated time (24 hours) at room temperature and under refrigeration. Linearity resulted in correlation coefficients greater than or equal to 0.999 for the evaluation and greater than or equal to 0.997 for impurities. We obtained a fluconazole recovery varying from 98 to 102% with an accuracy between 80 to 120% for impurities detection. The repeatability and reproducibility factor did not exceed a relative standard deviation of 2.0% for the evaluation and of 5.0% for the impurities, demonstrating the adequate robustness of the method. In addition, a short analysis execution time allowed the quick determination of the raw material quality.
Conclusion. We demonstrated that the fluconazole quantification method validated by high-performance liquid chromatography is sufficiently selective, precise, exact, linear, and robust to generate accurate analytical results under real conditions, including the tropical climate of Colombia.
Downloads
References
PubChem. Fluconazole. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://pubchem.ncbi.nlm.nih.gov/compound/3365
Tapia C. Mechanisms of action, adverse reactions and new antifungal agents. Medwave. 2005;5:e3548 https://doi.org/10.5867/medwave.2005.04.3548
Moncada DC, Montes M, Molina V, Velásquez JB, Gómez CI. Infección orofacial por Conidiobolus coronatus reporte de caso. Biomédica. 2016;36:15-22. https://doi.org/10.7705/biomedica.v36i2.2806
Rojas AE, Pérez JE, Hernández JS, Zapata Y. Análisis cuantitativo de la expresión de genes de resistencia a fluconazol en cepas de Candida albicans aisladas al ingreso de adultos mayores a una unidad de cuidados intensivos de Manizales, Colombia. Biomédica. 2020;40:153-65. https://doi.org/10.7705/biomedica.4723
Cortés JA, Ruiz JF, Melgarejo-Moreno LN, Lemos EV. Candidemia in Colombia. Biomédica. 2020;40:195-207. https://doi.org/10.7705/biomedica.4400
Nocua-Báez LC, Uribe-Jerez P, Tarazona-Guaranga L, Robles R, Cortés JA. Azoles de antes y ahora: una revisión. Rev Chil Infectol. 2020;37:219-30. https://doi.org/10.4067/s0716-10182020000300219
Sánchez-Hoyos F, Cárdenas A, Mercado-Camargo J, Domínguez-Moré G, Gómez-Estrada H. Validación de una metodología analítica USP por HPLC para la cuantificación de warfarina sódica en tabletas. Rev Colomb Cienc Quim Farm. 2016;45:470-83. https://doi.org/10.15446/rcciquifa.v45n3.62053
Samaniego JJ, Arias-Arroyo G. Desarrollo y validación de una metodología analítica por HPLC para la cuantificación simultánea de fenilefrina clorhidrato, paracetamol, salicilamida, cafeína y clorfeniramina maleato en tabletas. Rev Soc Quím Perú. 2016;82:196-207. Fecha de consulta: 12 de agosto de 2022. Disponible en: http://www.scielo.org.pe/scielo.php?script=sci_arttext&pid=S1810-634X2016000200010&lng=es&tlng=es
Romero-Díaz JA, Nuva-Paz L, López M, Ferrada C, Carballo C. Validación de una técnica por cromatografía líquida de alta resolución para la determinación del contenido de Mangiferina en hojas de Mangifera indica L. Rev Cuba Plantas Med. 2014;19:167-78.
Ulate-Molina R, Borbón-Alpízar H, Sibaja-Brenes JP, Vega-Guzmán I, Arguedas-González M. Validación de un método de detección mediante cromatografía líquida (HPLC-DAD) para la determinación de aloína en productos alimenticios elaborados a partir de sábila (Aloe vera). Uniciencia. 2019;33:13-26. https://doi.org/10.15359/ru.33-2.2
Sarria R, Campo V, Gallo J, Muñoz V. Validación de un método para el análisis de cocaína en muestras de orina empleando extracción en fase sólida (SPE) y cromatografía líquida de alta resolución (HPLC). Rev Cienc. 2018;21:81. https://doi.org/10.25100/rc.v21i1.6350
Bustillo P, Daza ML, Sierra-Martínez N. Validación de una metodología por HPLC en fase inversa para la determinación de Candesartan Cilexetil en tabletas recubiertas. Rev Colomb Cienc Quím Farm. 2014;43:55-68. https://doi.org/10.15446/rcciquifa.v43n1.45464
Unite States Pharmacopeia. USP Monographs, fluconazole. Fecha de consulta: 21 de marzo de 2022. Disponible en: https://doi.org/10.31003/USPNF_M33240_03_01
The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use. International conference on harmonisation of technical requirements for registration of pharmaceuticals for human use. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://database.ich.org/sites/default/files/Q2%28R1%29%20Guideline.pdf
Organización Panamericana de la Salud. Buenas prácticas de la OMS para laboratorios de control de calidad de productos farmacéuticos. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://www.paho.org/es/node/44617
Unite States Food and Drug Administration. Bioanalytical method validation. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://www.fda.gov/files/drugs/published/Bioanalytical-Method-Validation-Guidance-for-Industry.pdf
Unite States Pharmacopeia. U.S. Pharmacopeial Convention. 1225 Validation of compendial procedures. Fecha de consulta: 21 de marzo de 2022. Disponible en: https://doi.org/10.31003/USPNF_M99945_04_01
PubChem. 1,3-Di(1H-1,2,4-triazol-1-yl)benzene. Nih.gov. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://pubchem.ncbi.nlm.nih.gov/compound/1_3-Di_1H-1_2_4-triazol-1-yl_benzene
PubChem. 2-(4-fluorophenyl)-1,3-bis(1H-1,2,4-triazol-1-yl)propan-2-ol. Nih.gov. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://pubchem.ncbi.nlm.nih.gov/compound/134034
PubChem. 4-Defluoro-4-(1H-1,2,4-triazol-1-yl) fluconazole. Nih.gov. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://pubchem.ncbi.nlm.nih.gov/compound/11624578
United States Pharmacopeia. U.S. Pharmacopeial Convention. (621) Chromatography. Fecha de consulta: 12 de agosto de 2022. Disponible en: https://doi.org/10.31003/USPNF_M99380_01_01
Hitchcock SA, Pennington LD. Structure-brain exposure relationships. J Med Chem. 2006;49:7559-7583. https://doi.org/10.1021/jm060642i
Some similar items:
- Marisol García, Nohora Mendoza, Coordinadores del Programa de Diagnóstico de Malaria, Evaluation of the malaria diagnosis program in the national public laboratory network, Colombia, 1997-1999 , Biomedica: Vol. 22 No. 2 (2002)
- Catalina de Bedout, Julio Ayabaca, Ricardo Vega, Matilde Méndez, Axel R. Santiago, María Lucrecia Pabón, Angela Tabares, Myrtha Arango, Angela Restrepo, Vance Newell, Evaluation of Candida species' susceptibility to fluconazole with the disk diffusion method. , Biomedica: Vol. 23 No. 1 (2003)
- Tania Camacho, Fernando de la Hoz, Victor Cárdenas, Carmen Sánchez, Laura de Calderón, Ligia Pérez, Antonio Bermúdez, Incomplete surveillance of a dengue-2 epidemic in Ibagué, Colombia, 1995-1997. , Biomedica: Vol. 24 No. 2 (2004)
- Carlos Federico Molina, Catalina María Arango, Hernán Sepúlveda, Mercury contamination in breast milk of nursing mothers in gold mining municipalities of Antioquia, Colombia , Biomedica: Vol. 38 No. Sup.1 (2018): Suplemento 1, Enfermedades crónicas
- Isaura Torres, Juan E. Gallo , Oscar Mauricio Gómez , Álvaro Rúa-Giraldo , Juan G. McEwen , Ana María García , Gene expression profiles of ERG11, MDR1 and AFR1 in Cryptococcus neoformans var.grubbi from HIV patients , Biomedica: Vol. 42 No. 4 (2022)
- Ana Elisa Rojas, Leidy Yurany Cárdenas, María Camila García, Jorge Enrique Pérez, Expression of ERG11, ERG3, MDR1 and CDR1 genes in Candida tropicalis , Biomedica: Vol. 43 No. Sp. 1 (2023): Agosto, Micología médica
Copyright (c) 2023 Biomedica
This work is licensed under a Creative Commons Attribution 4.0 International License.
| Article metrics | |
|---|---|
| Abstract views | |
| Galley vies | |
| PDF Views | |
| HTML views | |
| Other views | |
