2012, Number 3
<< Back Next >>
Rev Cubana Farm 2012; 46 (3)
Validation of a liquid chromatographic method for determination of sulphadoxine and pyrimethamine in whole blood spotted on filter paper
Márquez FDM, Pabón VAL, López CCA, Blair TS
Language: English
References: 15
Page: 311-319
PDF size: 113.64 Kb.
ABSTRACT
Objective: to validate an analytical method for simultaneous determination and quantification of sulphadoxine and pyrimethamine in human blood dried onto filter paper, whose cost and analysis time can be reduced.
Methods: whole blood spotted on filter paper of a healthy volunteer and solutions of sulphadoxine-pyrimethamine standard mixture were used. HPLC separations were carried out on Agilent equipment using a LiChrospher
® column C18 with a mobile phase acetonitrile/0.1 M potassium phosphate buffer at pH 3.0 (1:1) for eight minutes under isocratic conditions. A flow rate of 0.7 mL/min, and a 20 mL volume injection were used. External standard method for quantitation of analytes was used.
Results: the HPLC method described for the simultaneous determination of sulphadoxine and pyrimethamine in 100 mL of whole blood spotted on filter paper has been found to be linear, precise, accurate and selective. In this method, the sample preparation is simple using liquid-liquid extraction, and HPLC with ultraviolet detection is used.
Conclusions: a simple, fast and sensitive method for determination of sulphadoxine and pyrimethamine in human blood dried onto filter paper was validated. This method can be used for the monitoring of both metabolites in pharmacokinetic and clinical studies.
REFERENCES
Edstein M. Quantification of antimalarial drugs. I. Simultaneous measurement of sulphadoxine, N4acetylsulphadoxine and pyrimethamine in human plasma. J Chromatogr. 1984;305:502-7.
Bergqvist Y, Eriksson M. Simultaneous determination of pyrimethamine and sulphadoxine in human plasma by high-performance liquid chromatography. Trans R Soc Trop Med Hyg. 1985;79:297-301.
Eljaschewitsch J, Padberg J, Schurmann D, Ruf B. High-performance liquid chromatography determination of pyrimethamine, dapsone, monoacetyldapsone, sulphadoxine and N-acetylsulfadoxine after rapid solid-phase extraction. Ther Drug Monit. 1996;18:592-7.
Edstein M. Quantification of antimalarial drugs. II. Simultaneous measurement of dapsone, monoacetyldapsone and pyrimethamine in human plasma. J Chromatogr. 1984;307:426-31.
Edstein MD, Lika ID, Chongsuphajaisiddhi T, Sabchareon A, Webster HK. Quantitation of Fansimef components (mefloquine + sulfadoxine + pyrimethamine) in human plasma by two high-performance liquid chromatographic methods. Ther Drug Monit. 1991;13:146-51.
Astier H, Renard C, Cheminel V, Soares O, Mounier C, Peyron F, et al. Simultaneous determination of pyrimethamine and sulfadoxine in human plasma by high-performance liquid chromatography after automated liquid-solid extraction. J Chromatogr B Biomed Appl. 1997;698(1-2):217-23.
Green MD, Mount DL, Nettey H. High-performance liquid chromatography assay for the simultaneous determination of sulphadoxine and pyrimetamine from whole blood dried onto filter paper. J Chromatog B. 2002;767;159-62.
Quattrocchi OA, De Andrizzi SA, Laba RF. Introducción a la HPLC Aplicación y Práctica. Buenos Aires: Artes Gráficas Farro, SA; 1992. p. 301-28.
Center for Drugs Evaluation and Research (CDER). Reviewer Guidance. Validation Chromatographic Methods. 5600 Fishers Lane, Rockville, Maryland 20857. November, 1994. Available from: http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Gui dances/UCM134409.pdf
US Food and Drug Administration. Guidance for industry: Q2B validation of analytical procedures: methodology. Rockville, MD: Nov, 1996. Available from: http://www.fda.gov/downloads/Drugs/GuidanceComplianceRegulatoryInformation/Gui dances/ucm073384.pdf
Eurachem. The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics; LGC (Teddington) Ltd.: Middlesex, United Kingdom, 1998. Available from: http://www.eurachem.org/guides/pdf/valid.pdf
Swartz ME, Krull IS. Validation of Chromatographic Methods. Pharmaceutical Technology Magazine. 1998;104:104-19.
Analytical Procedures and Method Validation: Highlights of FDA´s Draft Guidance. LC-GC [Internet]. 2001 [cited 2011 Aug 30];19(1). Available from: http://www.fda.gov/cder/guidance/2396dft.htm
Huber L. Validation of analytical methods: Review and Strategy. Waldbronn: Hewlett-Packard GmbH; 1998.
Castro M, Gascón S, Pujol M, Sans JM, Pla LV. Asociación Española de Farmacéuticos de la Industria. Validación de Métodos Analíticos. [Monografía]. Madrid: AEFI; 1989.