STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ALOGLIPTIN BENZOATE AND METFORMIN HYDROCHLORIDE IN TABLET DOSAGE FORM

Objective: A new simple, accurate, precise, economic and robust stability indicating RP-HPLC method has been developed and subsequently validated for the estimation of alogliptin and metformin in bulk and pharmaceutical dosage form.Methods: The HPLC separation was carried out by using hypersil BDS, C18 (250 x 4.6 mm, 5m.) column with a mobile phase comprising phosphate buffer and acetonitrile (48:52 % v/v) pH adjusted to 4.8 with orthophosphoric acid. The flow rate of the mobile phase was 1.0 ml/min and effluent was monitored at 210 nm using PDA detector. The retention time of alogliptin and metformin was 3.78 min and 2.78 min respectively. Forced degradation studies were conducted to know the stability of the drug samples under various stress conditions like acid, base, peroxide, and photolytic degradation according to ICH guidelines.Results: The results of this study showed excellent separation of the drug samples using developed method. The percentage recoveries were found 99.91 to 101.01% for alogliptin and 99.78-100.87% for metformin which is in the limits of acceptance. The calibration curve was plotted and the method was found to be linear over a range of 3-18 µg/ml and 125–750µg/ml of alogliptin and metformin respectively and regression data for calibration curve showed good linear relationship with r2= 0.9990 for the both alogliptin and metformin. In the study stability section, it was observed that there is no interference of the degradation products with drug samples.Conclusion: A new stability-indicating RP-HPLC method has been developed for estimation of alogliptin and metformin in bulk and pharmaceutical dosage form. The developed method was validated, and it was found to be simple, sensitive, precise, robust and it can be used for the routine analysis of alogliptin and metformin in both bulk and pharmaceutical dosage forms.Â

Silodosin oral films: Development, physico-mechanical properties and in vitro dissolution studies in simulated saliva

Sublingual film dosage forms for drugs used for fast symptomatic treatment have promise because they allow a rapid onset of action. The aim of this study was to prepare films of silodosin intended for sublingual administration for the symptomatic treatment of benign prostatic hyperplasia in men. Hydroxypropyl methylcellulose (HPMC) or hydroxypropyl methylcellulose acetate succinate (HPMC-AS) were used as film-forming polymers. The effects of the polymers and the surfactant tocopherol polyethylene glycol succinate (TPGS) on the physico-mechanical properties and dissolution behavior of the films in simulated saliva were investigated. The eight silodosin oral films developed (F1–F8) contained 8 mg silodosin per 6 cm2 film and HPMC or HPMC-AS in drug:polymer ratios of 1:5 or 1:3, while four also contained TPGS (0.5% w/w). The films were characterized using DSC, TGA, SEM, and PXRD and the mechanical properties were investigated by measuring tensile strength, elongation at break and Young's modulus. The mechanical properties of the films were dependent on the ratio of polymer used. The in vitro dissolution and drug release studies indicated that HPMC-AS films disintegrated more quickly than HPMC films. Silodosin was shown to be dispersed within the polymers. Despite silodosin being submicronized in the HPMC films, the dissolution and drug release rate (time for 80% release) from HPMC films was significantly faster than from HPMC-AS films. TPGS increased the drug release rate to a greater extent with HPMC than with HPMC-AS. The degree of saturation of formulation F4 was >1, which shows potential for improving oral absorption of silodosin.Peer reviewe

A Validated Stability Indicating RP-HPLC Method Development and Validation for Simultaneous Estimation of Aliskiren Hemifumarate and Amlodipine Besylate in Pharmaceutical Dosage Form

The present study describes the stability indicating RP-HPLC method for simultaneous estimation of aliskiren hemifumarate and amlodipine besylate in pharmaceutical dosage forms. The proposed RP-HPLC method was developed by using waters 2695 separation module equipped with PDA detector and chromatographic separation was carried on C-8 Inertsil ODS (150 × 4.6 mm, 5 µ) column at a flow rate of 1 mL/min and the run time is 10 min. The mobile phase consisted of phosphate buffer and acetonitrile in the ratio of 40 : 60% v/v and pH was adjusted to 3 with orthophosphoric acid and eluents were scanned using PDA detector at 237 nm. The retention time of aliskiren and amlodipine was found to be 3.98 and 5.14 min, respectively. A linearity response was observed in the concentration range of 30–225 µg/mL for aliskiren and 2–15 µg/mL for amlodipine, respectively. Limit of detection and limit of quantification for aliskiren are 0.161 µg/mL and 0.489 µg/mL and for amlodipine are 0.133 µg/mL and 0.404 µg/mL, respectively. The stability indicating method was developed by subjecting the drugs to stress conditions such as acid and base hydrolysis, oxidation, and photo- and thermal degradation and the degraded products formed were resolved successfully from the samples