ABSTRACT
Se presentan en este artículo los resultados obtenidos en desarrollo y validación de una metodología analítica para la cuantificación simultánea de piperacilina sódica y tazobactam sódico en inyectables para uso humano. El procedimiento consiste en una separación por cromatografía líquida de alta eficiencia (HPLC) en fase inversa empleando como fase móvil una mezcla de acetonitrilo e hidróxido de tetrabutilamonio 0,005M de pH 5,0 (31:69), una columna C18 a 38°C y detección a una longitud de onda de 220 nm. Se encontró que el método es selectivo, lineal y preciso. Estas características junto con su sencillez permiten que el método sea adecuado y conveniente para el objetivo propuesto. La robustez de la metodología fue también investigada. El método validado se aplicó para la determinación de las dos sustancias en un producto inyectable del mercado colombiano con registro sanitario del Instituto Nacional de Vigilancia y Control de Medicamentos y Alimentos (Invima).
A reverse phase high performance liquid chromatographic method was developed for the simultaneous quantitative assay of sodium piperaciline and sodium tazobactam. The method was validated and then applied to the quantitative determination assay of each of two substances A C18 column stabilized at 38 °C was used and the detection was performed at 220 nm. A mixture of acetonitrile and tetrabutylammonium hydroxide 0,005M pH 5,0 (31:69) was used as mobile phase. The method is selective, linear and shows a good repeatibility. The robustness was also verified. These properties besides their simplicities make it convenient for the objective proposed. The validated method was applied for the simultaneous assay of piperaciline and tazobactam in one market products with sanitary register at Instituto Nacional de Vigilancia y Control de Medicamentos y Alimentos (INVIMA).
ABSTRACT
Se presentan en este artículo los resultados del desarrollo y validación de una metodología analítica para la cuantificación de Candesartan Cilexetil en tabletas recubiertas para uso humano. El procedimiento consiste en una separación por cromatografía líquida de alta eficiencia en fase inversa y detector de arreglo de diodos, empleando como fase móvil una mezcla compuesta por un buffer de acetatos de pH 4,0 y acetonitrilo (30:70), una columna C18 a temperatura ambiente y detección a una longitud de onda de 306 nm. Se comprobó la selectividad, la precisión y la exactitud de la metodología. Estas características junto con su sencillez hacen el método adecuado y conveniente para el objetivo propuesto. La robustez de la metodología se investigó frente a la variación de algunas de las condiciones cromatográficas bajo las cuales se llevó a cabo la validación.
A reverse phase high performance liquid chromatographic method was developed for the quantitative assay of candesartan ciletexil in coated tablets for human use as hypotensor agent. The method was then validated for its quantitative determination assay in tablets as pharmaceutical specialties. A C18 column stabilized at room temperature was used and the detection was performed at 306 nm. A mixture of acetonitrile, acetate buffer pH 4,0 (30:70) was used as the mobile phase. The method is selective, linear and shows a good repeatability. The robustness was also studied. These properties besides the simplicity make the methodology convenient for the objective proposed.
ABSTRACT
A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.
Um método simples, rápido, econômico e confiável foi desenvolvido empregando a cromatografia líquida de alta eficiência para a determinação simultânea de etinilestradiol e drospirenona em comprimidos revestidos. O método foi realizado utilizando coluna LiChroCART® 100RP (125 x 4 mm d.i., 5 µm), a fase móvel constituída de acetonitrila:água, 50:50 (v/v) com vazão de 1,0 mL.min-1. A detecção foi realizada empregando fluorescência em λex= 280 nm e λem= 310 nm para o etinilestradiol e na região de UV em 200 nm para a drospirenona. O etinilestradiol e a drospirenona tiveram tempo de retenção de 4,0 e 5,7 min, respectivamente. O método foi validado de acordo com as diretrizes da USP 34. O método proposto apresentou vantagens sobre os relatados na literatura e pode ser considerado adequado para o controle de qualidade do etinilestradiol e da drospirenona em comprimidos revestidos.
Subject(s)
Chromatography, High Pressure Liquid , Contraceptives, Oral/analysis , Ethinyl Estradiol/pharmacokinetics , Tablets, Enteric-Coated , FluorescenceABSTRACT
La mangiferina se seleccionó como marcador en el control de calidad del ingrediente farmacéutico activo VIMANG® y sus formulaciones, que se han empleado como suplemento nutricional, cosmético y fitomedicamento. El trabajo tuvo como objetivo la validación del método electroforesis capilar para la determinación cuantitativa de mangiferina en la formulación farmacéutica tabletas VIMANG® 300 mg. Se evaluaron la especificidad, linealidad, exactitud y precisión. Los resultados obtenidos demostraron que el método fue específico, al no existir interferencias de los excipientes o sus productos de degradación. La linealidad mostró un coeficiente de correlación de 0,9979 en el intervalo de concentraciones estudiado. Los coeficientes de variación para la repetibilidad y la precisión intermedia fueron menores de 2 por ciento. La exactitud mostró un recobrado del 100,20 por ciento que no difiere significativamente de 100 por ciento En conclusión, el método validado es específico, lineal, preciso y exacto, y constituye una alternativa ventajosa al método cromatografía líquida de alta resolución establecido con anterioridad en el laboratorio
Mangiferin was selected as marker in the quality control of active principle VIMANG® and its formulations, which have been used as nutritional supplement, cosmetic, and phytomedication. This paper was aimed at validating the capillary electrophoresis method for the quantitative analysis of mangiferin in the pharmaceutical formulation 300 mg VIMANG® tablets. The specificity, linearity, accuracy and precision were assessed. The results showed the method specificity owing to lack of interference by the excipients or their degradation products. Linearity showed a correlation coefficient of 0,9979 in the studied concentration range. The variation coefficients for repeatability and intermediate precision were less than 2 percent. Accuracy reached a recovery rate of 100,20 percent that is not statistically different from 100 percent. It may be concluded that the validated method is specific, linear, precise and accurate and could be an advantageous alternative to the high resolution liquid chromatography method used at the lab setting
Subject(s)
Electrophoresis, Capillary/methods , Mangifera , Microscopy, UltravioletABSTRACT
Objective To develop an assay method for quantitative analysis of cocaine in rat's serum by high-performance liquid chromatography (HPLC). Method Serum samples (30?l) were extracted with 2% isoamyl alcohol and hexane. The organic phase was extracted with 0.1 mol/L HC1. The quantitative analysis was achieved by using a 5?m reversed-phase Kromasil CIS column with mobile phase of 0.04mol/ L phosphate buffer solution (containing 0.26 mmol/L tetrabutylammonium chloride , pH3.2) - acetonitrile (83:17). The wave length of the ultraviolet detection was performed at 235nm. Results The lowest limit of the detection limit was 25ng/ml. The recovery of the cocaine was 71 %. Conclusion The method is sensitive, simple and easy to perform.
ABSTRACT
Objective To improve a HPLOUV method for the determination of Tramadol hydrochlo-ride in human plasma. Method Alkalinized samples of plasma were extracted with dichloromethane. Tramadol and internai standard were analyzed on Elite C18 column (200mm?5.0mm, 5?m) with a acetoni-trile-phsphate buffer (pH6.5) (74:26, v/v) mobile phase and detedted at 220nm. Results The Calibra-tion plots in human plasma were linear (r=0.9984, n =5) from 10 to 800 ng/ml. The limit of detection was 10 ng/ml. For 20, 100, 400 ng/ml check samples, intra-run precisions (RSD) were 3.81% -5.44% and inter-run preceisions (RSD) were 3.95% -4.41% , respectively. The average recoveries were 89% , 96% and 92% for the low, middle and high check samples, respectively. Conclusion The improved ana-lytical method for Tramadol hydrochloride was found to be sensitive, simple and rapid, suitable for applica-tion in forensic toxicological analysis and routine determination of numerous samples.