RESUMEN
Two chromatographic methods (high performance thin layer chromatography (HPTLC) and high performance liquid chromatography-diode array detector (HPLC-DAD)), were addressed for the analysis of a mixture consisted of phenylephrine hydrochloride and ibuprofen in two forms bulk and their combined dosage form. This binary mixture is considered to be a challenging one as the two drugs differ greatly in their chemical and physical properties. Not only this affects their simultaneous analysis, but also hinders their simultaneous extraction from biological fluids as plasma. That is the reason the literature lacks any report for the simultaneous extraction and analysis of these drugs from biological fluids. The concentration ranges of both drugs were 0.1-2.5 µg/spot and 0.1-100 µg/mL by HPTLC and HPLC, respectively. Not only was the HPLC-DAD method applied to the investigated drugs determination in pharmaceutical preparations, but also in spiked human plasma. Extensive study was conducted to optimize their simultaneous extraction from plasma as it was a crucial step for the in vivo analysis. The results obtained by proposed methods and a reference one were statistically comparable by analysis of variance test. No significant difference was recorded between the mean percent levels determined by the proposed methods and the reference one.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Cromatografía en Capa Delgada/métodos , Ibuprofeno/análisis , Fenilefrina/análisis , Combinación de Medicamentos , Humanos , Ibuprofeno/sangre , Ibuprofeno/química , Ibuprofeno/aislamiento & purificación , Límite de Detección , Modelos Lineales , Fenilefrina/sangre , Fenilefrina/química , Fenilefrina/aislamiento & purificación , Reproducibilidad de los Resultados , Extracción en Fase Sólida , ComprimidosRESUMEN
Background: A validated method based on capillary zone electrophoresis coupled with a diode array detector (CZE-DAD) was investigated for analyzing binary mixture of ibuprofen (IBU) and phenylephrine (PHE) in their bulk and combined dosage form. Objective: This binary mixture is a challenging one as IBU is acidic and PHE is alkaline, which may affect their simultaneous analysis using CZE. The literature lacks any CZE report for IBU and PHE simultaneous analysis. Methods: Fused silica capillary (85 cm × 75 µm id) was used, and the electrolyte was a 50 mM borate buffer adjusted to pH 11 with 0.5 M NaOH. Results: The concentration ranges were 5-200 and 5-100 µg/mL for IBU and PHE, respectively, using CZE. High efficiency was achieved (N > 92990). Reasonable migration time (tm) was attained (tm< 8.5 min). Conclusions: Although the results obtained by the proposed CZE method and reported HPLC method were statistically comparable, the proposed method showed lower linearity ranges, higher efficiency, and a more reasonable run time. Highlights: CZE-DAD was used for the analysis of IBU and PHE in bulk and tablets, as no report was found for their determination using CZE. Binary mixture is challenging due to differences in chemical and physical properties. A detailed discussion of electrophoretic parameters optimization is included. Confirmation of peak purity was attained using DAD.
Asunto(s)
Electroforesis Capilar/instrumentación , Electroforesis Capilar/métodos , Ibuprofeno/análisis , Fenilefrina/análisis , Cromatografía Líquida de Alta Presión , ComprimidosRESUMEN
A simple and rapid high-performance liquid chromatographic method for the determination of proquazone (PQZ) and its major metabolite, m-hydroxyproquazone, in spiked human plasma and urine was developed. Plasma samples were purified using acetonitrile as a protein precipitant, while urine samples were diluted only with the mobile phase and filtered prior to injection. Samples containing the parent compounds and glafenine (internal standard) were eluted from a reversed-phase C8 column using acetonitrile-0.025 M sodium acetate (60 + 40) adjusted to pH 5 as the mobile phase and detected at 234 nm. Peak area ratios of the analytes versus internal standard were used for calibration. The mean recoveries from plasma and urine samples spiked with PQZ and its m-hydroxy metabolite ranged from 97.87 to 103.88%. The relative standard deviation for the within- and between-day analyses were < 4%. The proposed method was applied for the assay of PQZ in laboratory-made tablets.
Asunto(s)
Análisis Químico de la Sangre/métodos , Cromatografía Líquida de Alta Presión/métodos , Quinazolinas/análisis , Quinazolinas/sangre , Quinazolinas/orina , Urinálisis/métodos , Calibración , Química Farmacéutica/métodos , Cromatografía/métodos , Cromatografía Liquida/métodos , Relación Dosis-Respuesta a Droga , Modelos Químicos , Estándares de Referencia , Comprimidos , Factores de TiempoRESUMEN
A simple, rapid and sensitive voltammetric method for the determination of floctafenine (FFN) and metopimazine (MPZ) was developed. Well-defined cathodic waves were obtained for both drugs in Britton-Robinson buffer pH 9.0 using the differential-pulse mode at the hanging mercury drop electrode (HMDE). The current-concentration relationship was found to be linear over the ranges 0.4-3.6 and 0.4-2.4 microg ml(-1) for FFN and MPZ, respectively. The quantification of the two drugs in their pharmaceutical formulations was carried out using the proposed voltammetric method and compared with spectrophotometric analysis data. The mechanisms of the electrode reactions for the two drugs were proposed.
Asunto(s)
Antiinflamatorios no Esteroideos/química , Antieméticos/química , Ácidos Isonipecóticos/química , ortoaminobenzoatos/química , Tampones (Química) , Electroquímica/instrumentación , Electroquímica/métodos , Electrodos , Concentración de Iones de Hidrógeno , Estructura Molecular , Preparaciones Farmacéuticas/análisis , Sensibilidad y Especificidad , Espectrofotometría , Factores de TiempoRESUMEN
The stripping voltammetric behaviour of buspirone hydrochloride (BUS) and piribedil (PIR), as models of pyrimidine-containing compounds, was studied using a hanging mercury drop electrode (HMDE). A sensitive adsorptive stripping voltammetric method for determination of such drugs is described. The voltammetric peaks were obtained at -1.23 and -1.22 V for BUS and PIR. respectively, which correspond to the reduction of the azomethine group of pyrimidine ring in Britton-Robinson buffer (pH 7). Factors such as pH of supporting electrolyte, accumulation potential and time and instrumental parameters were optimized. Calibration plots and regression data validation, accuracy, precision, limits of detection, limits of quantification, and other aspects of analytical merit are presented. The applicability of the method was evaluated through determination of BUS and PIR in tablet dosage forms. A preliminary study of the analysis of plasma samples, spiked with the investigated drug, after a simple extraction procedure is described.
Asunto(s)
Compuestos Azo/análisis , Compuestos Azo/farmacocinética , Pirimidinas/análisis , Pirimidinas/farmacocinética , Adsorción , Buspirona/análisis , Buspirona/farmacocinética , Electroquímica , Naftalenosulfonatos/análisis , Naftalenosulfonatos/química , Naftalenosulfonatos/farmacocinética , Preparaciones Farmacéuticas/análisis , Preparaciones Farmacéuticas/metabolismo , Piribedil/análisis , Piribedil/farmacocinética , Tiosemicarbazonas/análisis , Tiosemicarbazonas/química , Tiosemicarbazonas/farmacocinéticaRESUMEN
The British Pharmacopoeia defines 2-aminopyridine (2-AP) as a potential impurity in piroxicam (PX) and tenoxicam (TX). Selective spectrofluorimetric determination of 2-AP in PX and TX, within or near the pharmacopoeial level, 0.2%, was developed, based on the measurement of the native fluorescence either in aqueous 0.1N sulfuric acid or in dioxane. Accordingly, this approach was followed for confirming purity of PX and TX in bulk and pharmaceutical preparations. The study was also extended to include simultaneous determinations of PX/2-AP and TX/2-AP systems based on selective fluorescence measurements in the cited solvents.