A simple, specific and stability-indicating reversed phase high performance liquid chromatographic method was developed for the quantitative determination of asenapine in tablet dosage form. A SunFire C18, 5 μm column having 250×4.6 mm i.d. in isocratic mode, with mobile phase containing 0.02 M potassium dihydrogen phosphate: acetonitrile (95:05, v/v, pH 3.5 adjusted with 1% o-phosphoric acid) was used. The flow rate was 1.0 mL min−1 and effluents were monitored at 232 nm. The retention time of asenapine was 5.51 min. The linearity for asenapine was in the range of 0.1–20 μg/ml. The recoveries obtained for asenapine were 98.31–101.51%. Asenapine stock solutions were subjected to acid and alkali hydrolysis, chemical oxidation, sunlight and dry heat degradation. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time values. Stressed samples were assayed using developed LC method. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of asenapine in tablet dosage form.
A sensitive, precise, robust and accurate high performance thin layer chromatographic method was developed and validated base on ICH Q2 (R1) guideline for the simultaneous estimation of Perindopril erbumine, Indapamide and Amlodipine besylate in bulk and combined Triplixam marketed tablet dosage formulation. Pre‐coated silica gel aluminum plate 60 F254 was selected as the stationary phase and dichloromethane: methanol: toluene: glacial acetic acid (7: 1: 2: 0.1, v/v/v/v) was used as developing mobile phase. The common detection wavelength for Perindopril erbumine, Indapamide and Amlodipine besylate was carried out at 215 nm. The method was validated for linearity, precision, accuracy, and robustness, limit of detection and limit of quantitation as per ICH parameters. The correlation coefficient (r2) of Perindopril erbumine, Indapamide and Amlodipine besylate were found to be 0.9987, 0.9987 and 0.9996, respectively. The mean of percentage recovery of Perindopril erbumine, Indapamide and Amlodipine besylate were found to be 99.38‐101.81, 100.61‐102.68 and 99.87‐101.95%, respectively. The proposed thin layer chromatography method has potential qualitative as well as quantitative applications for simultaneous estimation of Perindopril erbumine, Indapamide and amlodipine besylate in bulk and pharmaceutical dosage form.
Background
Extensive literature review revealed that no RP–LC method has been developed for simultaneous estimation of EMPA, LINA and MET in combined dosage form. This is a newer combination approved by USFDA on 4th June 2019 and it is launch in the United State Market on 27th January 2020.
Result
A simple, sensitive, specific, precise and accurate reverse phase—high performance liquid chromatography (RP- HPLC) method has been developed for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. Phenomenex C18 column (250 mm × 4.6 mm, 5 µm) was used as stationary phase for chromatographic separation through isocratic elution using Acetonitrile: Methanol: Water in a ratio (27: 20: 53, v/v/v) pH 4 adjusted with 1% Ortho-phosphoric acid as mobile phase at flow rate 1 ml/min. PDA detector was used for simultaneous analysis of all three drugs at common wavelength 223 nm and the each injection volume was 20 µl. The linearity range for Empagliflozin, Linagliptin and Metformin HCl was found to be 0.5–5 µg/ml, 0.25–2.5 µg/ml, and 50–500 µg/ml, respectively. The retention time for Empagliflozin, Linagliptin and Metformin HCl was found to be 14.5 min, 3.4 min and 2.01 min, respectively. The percentage (%) recovery was found to be 99.98–100.81% for Empagliflozin, 99.33–100.57% for Linagliptin and 100.65–101.35% for Metformin HCl respectively.
Conclusion
As per the international Conference on Harmonisation (ICH) Q2 (R1) guideline, proposed RP–LC method validation has been carried out. The proposed RP–LC method was repeatable and selective as per statistical analysis and it can be use for simultaneous estimation of Empagliflozin, Linagliptin and Metformin HCl in bulk and synthetic mixture. The proposed method might be applied for simultaneous estimation of all three drugs in pharmaceutical formulation.
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