Atorvastatin 1) is a synthetic lipid lowering agent which inhibits HMG-CoA reductase and amlodipine 2) is a calcium antagonist drug effective in hypertension and angina pectoris. The combination drug product of atorvastatin (ATV) and amlodipine (AML) has recently been introduced in the market; co-administration of AML with ATV demonstrated statistically significant dose-related reductions in systolic blood pressure (SBP), diastolic blood pressure (DBP) and LDL-C in patients with co-morbid hypertension and dyslipidemia. 3)Chemically ATV is [R-(R*,R*)]-2-(4-fluorophenyl)-b, dihydroxy-5-(1-methylethyl)-3-phenyl-4-[(phenylamino) carbonyl]-1H-pyrrole-1-heptanoic acid, calcium salt (2 : 1) trihydrate 4) and AML is 2-[(2-Aminoethoxy)-methyl]-4-(2-chlorophenyl)-1,4-dihydro-6-methyl-3,5-pyridinedicarboxylic acid 3-ethyl 5-methyl ester. 5)Stability testing forms an important part of the process of drug product development. The purpose of stability testing is to provide evidence on how the quality of a drug substance or drug product varies with time under the influence of a variety of environmental factors such as temperature, humidity, and light, and enables recommendation of storage conditions, retest periods, and shelf lives to be established. The two main aspects of drug product that play an important role in shelf life determination are assay of active drug, and degradation products generated, during the stability study. The assay of drug product in stability test sample needs to be determined using stability indicating method, as recommended by the International Conference on Harmonization (ICH) guidelines 6) and USP-26. 7) Although stability indicating methods have been reported for assay of various drugs in drug products, most of them describe assay procedures for drug products containing only one active drug substance. Only few stability indicating methods are reported for assay of combination drug products containing two or more active drug substances. The objective of this work was to develop a simple, precise and rapid analytical LC procedure, which would serve as stability indicating assay method for combination drug product of ATV and AML.Both methods have been reported for simultaneous determination of ATV and AML, but these methods lack stability indicating nature. None of the reported analytical procedures describe a stability indicating method for simultaneous determination of ATV and AML in presence of their degradation products. This manuscript describes the development and validation of a stability indicating isocratic reversed-phase HPLC method for simultaneous determination of ATV and AML in presence of their degradation products as per ICH guidelines. The study describes development and subsequent validation of a stability indicating reverse-phase HPLC method for the simultaneous estimation of atorvastatin (ATV), and amlodipine (AML) from their combination drug product. The proposed RP-HPLC method utilizes a Lichrospher ® 100 C 18 , 5 m mm, 250 mm؋4.0 mm i.d. column, at ambient temperature, optimum ...
A simple, precise, and rapid stability-indicating reversed-phase column liquid chromatographic (RP-LC) method has been developed and subsequently validated for simultaneous estimation of simvastatin (SIM) and ezetimibe (EZE) from their combination drug product. The proposed RP-LC method utilizes a LiChrospher 100 C18, 5 m, 250 4.0 mm id column at ambient temperature; optimum mobile phase consisting of acetonitrilewatermethanol (60 + 25 + 15, v/v/v) with apparent pH adjusted to 4.0 0.1; mobile phase flow rate of 1.5 mL/min; and ultraviolet detection at 238 nm. SIM, EZE, and their combination drug product were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method is specific for the estimation of SIM and EZE in the presence of degradation products. The described method was linear over the range of 180 and 380 g/mL for SIM and EZE, respectively. The mean recoveries were 99.17 and 100.43 for SIM and EZE, respectively. The intermediate precision data were obtained under different experimental conditions, and the calculated value of the coefficient of variation was found to be less than the critical value. The proposed method can be useful in the quality control of bulk manufacturing and pharmaceutical dosage forms.
Three simple and sensitive spectrophotometric, difference spectroscopic, and liquid chromatographic (LC) methods are described for the determination of cefixime. The first method is based on the oxidative coupling reaction of cefixime with 3-methyl-2-benzothiazolinon hydrazone HCl in presence of ferric chloride. The absorbance of reaction product was measured at the maximum absorbance wavelength (max), 630 nm. The difference spectroscopic method is based on the measurement of absorbance of cefixime at the absorbance maximum, 268 nm, and minimum, 237 nm. The measured value was the amplitude of maxima and minima between 2 equimolar solutions of the analyte in different chemical forms, which exhibited different spectral characteristics. The conditions were optimized, and Beer's law was obeyed for cefixime at 1 to 16 μg/mL and 10 to 50 μg/mL, respectively. The third method, high-performance LC, was developed for the determination of cefixime using 50 mM potassium dihydrogen phosphate (pH 3.0)methanol (78 + 22, v/v) as the mobile phase and measuring the response at λmax 286 nm. The analysis was performed on a Lichrospher RPC18 column. The calibration curve was obtained for cefixime at 5 to 250 μg/mL, and the mean recovery was 99.71 ± 0.01%. The methods were validated according to the guidelines of the U.S. Pharmacopoeia and also assessed by applying the standard addition technique. The results obtained in the analysis of dosage forms agreed well with the contents stated on the labels.
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