SIMULTANEOUS DETERMINATION OF METFORMIN, LINAGLIPTIN IN JENTADUETO AND METFORMIN, SAXAGLIPTIN IN KOMBIGLYZE BY LC-MS METHOD
Keywords:Linagliptin, LC-MS, Method development, Metformin, Saxagliptin, Validation
Objective: The objective of the present investigation was to develop a novel, simple and economic method for the determination of metformin (MET), linagliptin (LIN) and saxagliptin (SAX) in jentadueto and kombiglyze sample by employing the liquid chromatography and mass spectrometric method for estimation in bulk and pharmaceutical dosage form in presence of degradation products.
Methods: The chromatographic separation was achieved by using the mobile phase composition of methanol and ammonium acetate buffer pH 4.5 (85:15 % v/v) on the Hypurity advance C-18 column at a flow rate of 0.5 ml/min. Ion signals m/z 130.10/70.10, 473.10/420.40 and 316.30/180.20â€ for metformin, linagliptin and saxagliptin respectively measured in positive ion mode. The detailed validation of the method was performed as per ICH guidelines.
Results: The results of all validation parameters found within acceptance limits. The linearity of the drugs was found to be in the concentration range of 50â€“5000 ng/ml for all the drugs. Accuracy of the drugs was found to be from 94-102% and precision was found 4.67% RSD for all three drugs. The validated method was employed for the determination of drugs in the formulation and also determined the drugs in the presence of degradation products under stress conditions.
Conclusion: The method was developed and validated as per guidelines. Hence, this method can be used for the simultaneous determination of metformin, linagliptin and metformin, saxagliptin in bulk and combined dosage forms.
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