RESUMEN
The aim of this study is to develop and validate two simple spectrophotometric methods for simultaneous determination of metoprolol succinate (MET) and olmesartan medoxomil (OLM) in tablet form. Method (I) was area under the curve (AUC) method. This approach involved the measuring of the area over a variety of wavelengths. Two wavelength ranges; 213-230 nm and 244-266 nm were chosen for determination of MET and OLM, respectively. Method (II) was ratio difference spectrophotometricmethod. For determination of MET, the ratio spectra were generated using 15 µg/mL OLM as a divisor then the peak to trough amplitudes between 221 nm and 245 nm were displayed versus the corresponding concentrations of MET. For determination of OLM, the peak-to-peak amplitudes between 247 and 293 nm were chosen and found to be directly proportional to OLM concentrations using 15 µg/mL MET as a divisor. The linearity ranges were 2-30 µg/mL and 2-25 µg/mL for MET and OLM, respectively. The assay results showed good mean %recovery ± SD as well as good agreement with that of the reported method. The developed methods were validated according to ICH guidelines. The developed methods are accurate, precise, eco-friendly and could be applied successfully to estimate OLM and MET in their combined dosage form.
Asunto(s)
Metoprolol , Olmesartán Medoxomilo , Espectrofotometría/métodosRESUMEN
For the first time a spectrofluorimetric method had been achieved for the concurrent analysis of metoprolol succinate (MET) and olmesartan medoxomil (OLM). The approach depended on assessing the first order derivative (1D) of the synchronous fluorescence intensity of the two drugs in aqueous solution at Δλ of 100 nm. The amplitudes of 1D at 300 nm and 347 nm were measured for MET and OLM, respectively. The linearity ranges were 100-1000 ng/mL and 100-5000 ng/mL for OLM and MET, respectively. This approach is uncomplicated, repetitive, quick, and affordable. The results of analysis had been statistically verified. The validation assessments were carried out following the recommendations of The International Council for Harmonization (ICH). This technique could be employed to assess marketed formulation. The method was sensitive with limits of detection (LOD) of 32 ng/ml and 14 ng/mL for MET and OLM, respectively. Limits of quantitation (LOQ) were 99 ng/ml for MET and 44 ng/mL for OLM. So it can be applied to determine both drugs in spiked human plasma within the linearity ranges of 100-1000 ng/mL for OLM and 100-1500 ng/mL for MET.
Asunto(s)
Metoprolol , Humanos , Olmesartán Medoxomilo/química , Espectrometría de Fluorescencia , Preparaciones FarmacéuticasRESUMEN
For determination of amlodipine besylate (AML) and olmesartan medoxomil (OLM) at the same time, four UV chemometric spectrophotometric techniques were created and tested in accordance with ICH standards. Method (I) was absorption subtraction method (ASM) using two wavelengths, one of which was of AML at 365 nm and the other was the isoabsorptive point of both drugs at 237 nm. Method (II) was ratio subtraction method (RSM) for determination of OLM at λmax = 254 nm by taking the ratio spectrum and subtracting the constant values using 10 µg/mL of AML as a divisor in combination with extended ratio subtraction method (ERSM) to determine AML at λmax = 239 nm using 10 µg/mL OLM as a divisor. Method (III) was dual wavelength method; the wavelengths used to determine OLM were 221 nm and 235 nm, while those used to determine AML were 246 nm and 259 nm. Method (IV) was the second order derivative (2D) spectrophotometric method at 219 nm for OLM and 227 nm for AML. The proposed approaches were used to achieve linearity in the concentration range of 2-25 µg/mL for both drugs. The approaches were found to be uncomplicated, reproducible, efficient, and cost-effective as well as they were successfully used to determine the cited drugs in both laboratory samples and commercial pharmaceutical formulations.
Asunto(s)
Amlodipino , Olmesartán Medoxomilo , Espectrofotometría , ComprimidosRESUMEN
Two simple chemometric spectrophotometric methods; isosbestic point and dual wavelength methods were developed, validated and applied to the determination of metoprolol succinate in presence of amlodipine besylate in their binary mixtures and in combined tablet formulation while amlodipine besylate was determined by direct spectrophotometry at λ = 365 nm within linearity range of 2-25 µg/mL. The mean percentage recovery ± SD was 99.921 ± 0.089 for amlodipine besylate. Two proposed chemometric spectrophotometric methods were developed for the spectral resolution of metoprolol succinate in presence of amlodipine besylate without preliminary separation with a linearity range of 2-30 µg/mL metoprolol succinate. The first method depended on measuring the absorbance at the isosbestic point at λ = 226 nm. The mean percentage recovery ± SD was 100.110 ± 0.249 for metoprolol succinate. The second method was dual wavelength method, metoprolol could be determined alone using the absorbance difference between 226 nm and 248.7 nm where the absorbance difference was zero for amlodipine at these two wavelengths. The mean percentage recovery ± SD was 99.734 ± 0.438 for metoprolol succinate using dual wavelength method. The developed methods were validated as per ICH guidelines and were successfully applied to analysis of cited drugs in their synthetic tablet formulation. The results obtained by the developed methods were statistically compared to those obtained by a reported one using t-test and F- test. Good agreement was observed.