Objective: The combination of hydrocodone and ibuprofen is prescribed to temporarily relieve severe pain. A new selective, precise and accurate stability indicating reverse phase high performance liquid chromatography (RP-HPLC) technique was developed for identification and estimation of hydrocodone and ibuprofen in tablets. Methods: The analysis of hydrocodone and ibuprofen was executed on phase Zodiac C18 (250 × 4.6 mm, 5 μm) column with sodium dihydrogen phosphate (0.1M, pH5.0) and methanol (60:40, v: v) as a mobile phase with a flow rate of 1.0 ml/min. The detection and measurement was done at 234 nm. The stability of hydrocodone and ibuprofen was examined under different conditions recommended by ICH, including alkaline, acidic, neutral, oxidative, photolytic and thermal. Results: Hydrocodone and ibuprofen are eluted at 4.019 min and 4.999 min, respectively. The assay method was linear (range: 3.75-11.25 µg/ml and 100-300 μg/ml) with R2values of 0.9996 and 0.9999 for hydrocodone and ibuprofen, respectively. Method was accurate (recovery: 99.65% and 99.37% for hydrocodone and ibuprofen, respectively), precise (RSD: 0.262% and 0.261% for hydrocodone and ibuprofen, respectively), selective and robust. In degradation studies, peaks of degradants did not interfere with the peaks of hydrocodone and ibuprofen. This validated method was applied to assay the content of hydrocodone and ibuprofen in tablets. Conclusion: This method can be opted in the routine quality control test of fixed dose tablet combination comprising of hydrocodone and ibuprofen.
Dovato tablets (lamivudine and dolutegravir combination) are full therapy regimen for the Type 1 human immunodeficiency virus (HIV-1) infection in adults without history of antiretroviral therapy. The aim of present research focused on development of validated stability indicating method for the quantification of lamivudine and dolutegravir in combined dosage form.The separation was achieved on a Cosmicsil C18 column. The mobile phase consisted of 0.1% orthophosphoric acid (pH 3.5) – acetonitrile (50:50, v/v). Photodiode array detector was used to detect the analytes at 258 nm. The method performance was validated in compliance with the recommendations of the International Conference on Harmonization.The method was validated with selectivity, limit of detection (0.262 μg/ml for lamivudine and 0.238 μg/ml for dolutegravir), linearity (150-450 μg/ml for lamivudine and 25-75 μg/ml for dolutegravir), limit of quantification (0.874 μg/ml for lamivudine and 0.793 μg/ml for dolutegravir), accuracy (percent recovery was nearer to 100%), precision (percent relative standard deviation was less than 2.0%) and robustness (system suitability values are within limits). The stability indicating method was performed by under the various stress conditions. Degradants did not interfere with lamivudine and dolutegravir detection. The developed method can suggest that quantification of lamivudine and dolutegravir in quality control of analytical laboratories.
Objective: The objective of the study was to develope a stability indicating high-performance liquid chromatographic (HPLC) method for simultaneous assay of pentazocine and naloxone in bulk and tablets. Methods: Pentazocine and naloxone were analyzed on Dionex C18 column using 0.1M K2HPO4 buffer (pH 4.0) and methanol (60:40, v/v) as the mobile phase. The concentration of pentazocine and naloxone was quantified by photodiode array detector set at 248 nm. The method was validated in compliance with ICH rules. Pentazocine and naloxone tablet formulation was subjected to forced degradation such as acid, neutral and alkali hydrolysis, oxidation, photo, and thermal degradation. Results: The method was linear, with R2=0.9999 in the concentration range 100–300 μg/ml for pentazocine and R2=0.9995 in the concentration range 1–3 μg/ml for naloxone. The level of detection and quantification was 0.097 μg/ml and 0.322 μg/ml for pentazocine and 0.0073 μg/ml and 0.0243 μg/ml for naloxone, respectively. The degraded products are resolved well from pentazocine and naloxone with significantly different retention time values. From validation results, it was proved that the method is selective, precise, robust, and accurate for the estimation of pentazocine and naloxone simultaneously. Conclusion: The developed stability-indicating HPLC method can be applied for quantitative determination of pentazocine and naloxone in tablets.
Aim: To Perform Simultaneous Determination of Saxagliptin, Dapagliflozin and Metformin Tablet dosage form developed in a simple, Accurate, precise manner. Method: Agilent C18 150 x 4.6mm, 5m. Mobile phase containing 0.1% OPA: Acetonitrile taken in the ratio 50:50 was pumped through column at a flow rate of 1.0 ml/min used for the development of chromatogram. Buffer used in this method was 0.1% OPA. Temperature was maintained at 30°C. Optimized wavelength selected was 260nm. Results and Conclusion: Retention time of Saxagliptin, Dapagliflozin and Metformin were found to be 2.253 min, 2.720 min, 3.276 min respectively. % RSD of the Saxagliptin, Dapagliflozin and Metformin were and found to be 0.8, 0.2 and 0.6. % Recovery was obtained as 99.60%, 100.07% and 99.95% for Saxagliptin, Dapagliflozin and Metformin respectively. LOD, LOQ values obtained from regression equations of Saxagliptin, Dapagliflozin and Metformin were 0.06, 0.12, 9.61 and 0.17, 0.36, 29.31 respectively. Regression equation of Saxagliptin is y = 40882x + 889.2, Dapagliflozin is y = 47904x + 3897 and Metformin is y = 4530.x + 35785. Retention times were decreased and that run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.
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