Development and Validation of a Stability-Indicating Assay Method for Simultaneous Determination of Perindopril and Indapamide in Combined Dosage Form by Reversed-Phase High-Performance Liquid Chromatography

Abstract

An approach of forced degradation study was successfully applied for the development of a stability-indicating assay method for simultaneous determination of perindopril and indapamide in a formulation in the presence of its degradation products. The method showed adequate separation of perindopril and indapamide from their associated main impurities and degradation products. Separation was achieved on an XTerra<sup/> RP18, 5 µm, 150 4.6 mm id column at 55°C by using the mobile phase NaH2PO4 buffer (pH 2.0; 0.005 M)acetonitrile (75 + 25, v/v ) at a flow rate of 1 mL/min and UV detection at 215 nm. Comprehensive stress testing of perindopril and indapamide was carried out according to the International Conference on Harmonization (ICH) guideline Q1A (R2). The specificity of the method was determined by assessing interference from the placebo and by stress testing of the drug (forced degradation). The drug was subjected to acid hydrolysis, base hydrolysis, oxidation, dry heat, and photolysis to apply stress conditions. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method was specific for determination of perindopril and indapamide in the presence of degradation products. The method was validated in terms of linearity, precision, accuracy, specificity, robustness, and solution stability. The linearity of the proposed method was investigated in the range of 2456 µg/mL (r2 = 0.9993) for perindopril and 7.517.5 µg/mL (r2 = 0.9992) for indapamide. Degradation products produced as a result of stress studies did not interfere with the detection of perindopril and indapamide, and the assay can thus be considered stability indicating.

Optimized Chitosan/Anion Polyelectrolyte Complex Based Inserts for Vaginal Delivery of Fluconazole: In Vitro/In Vivo Evaluation

“…All the prepared vaginal inserts exhibited acceptable drug content, ranging from 95 ± 0.029% to 102 ± 0.057%. These results are in accordance with the pharmacopeial limit of (85–115%) [14,32]. Friability values for all inserts ranged between 1.91 ± 1.49% and 6.34 ± 2.91%, Table 1, which is in accordance with the acceptable range for lyophilized vaginal inserts previously reported in the literature [16].…”

Method development and validation of HPLC tandem/mass spectrometry for quantification of perindopril arginine and amlodipine besylate combination in bulk and pharmaceutical formulations

“…Since no sensitive method for quantification of the perindopril arginine and amlodipine besylate as combination in bulk drugs or pharmaceuticals using LC-MS technique has been reported, the validated RP-UPLC/ESI-MS/MS assay method was developed which yields highly reproducible chromatographic results when quantifying perindopril and amlodipine and provides an accurate and precise assay for analyzing combined dosage form of bulk drugs and tablet formulations. Moreover, currently available methods ( 9 10 11 12 ) are developed either for each individual drug or their combination with other drug molecules and also they are time consuming with laborious sample preparation, so there is a need for developing a fully automated online method for the determination of perindopril and amlodipine.…”

“…Most of the earlier methods are not ideal since they are time-consuming, have high limits of detections, use of surplus organic solvents, laborious sample preparation, involve expensive instrumentation and long chromatographic run times ( 9 10 11 12 ). In recent years, reverse phase ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (RP-UPLC-ESI-MS/MS) studies have emerged in the pharmaceutical field as a very crucial tool based on the reality that, studies has been used for the successful characterization of the in vitro behavior of drugs ( 13 ).…”

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“…(Research Article) spectrophotometry 5,6 , LC with tandem MS 7,8 , HPLC 9,10, and HPTLC [11][12] . Indapamide (IND) is chemically 4-chloro -N-[(2RS)-2-methyl -2, 3dihydro -1H -indol -1-yl] -3sulfamoylbenzamide Fig.…”