Sitagliptin

Sitagliptin chemically is (3R) -3-amino-1-[3- (trifluoromethyl)-6,8-dihydro-5h- [1,2,4] triazolo [3,4-c] pyrazin-7-yl]-4-(2,4,5-trifluorophenyl) butan-1-one (Fig. 1), an oral anti-diabetic agent that blocks Dipeptidyl peptidase-4 (DPP-4) activity. Sitagliptin increased incretin levels (GLP-1 and GIP) which inhibit glucagon release, in turn decreases blood glucose, but more significantly increases insulin secretion. The present work describes development and validation of a new simple, accurate, precise and stability indicating HPTLC method for the determination of sitagliptin in tablet dosage form. The chromatographic separation was achieved by using Toluene: Ethyl acetate: Methanol (3: 6: 1 v/v/v) as mobile phase and UV detection at 238 nm. The developed method was validated with respect to linearity, accuracy, precision, limit of detection, limit of quantitation and robustness as per ICH guidelines. The drug was subjected to stress condition of acid hydrolysis, alkali hydrolysis, photolysis, thermal degradation. Results found to be linear in concentration range of 100-500 ng/band. The developed method can be used for the quantification of bulk drug as well as in formulation. Keywords: Sitagliptin, HPTLC, Degradation Studies

A selective, robust, economic and short method was developed for the simultaneous estimation of the Ertugliflozin (EGZ) and Sitagliptin (SGP) in Tablet dosage form. Chromatogram was run through  X-bridge c18 50 x 2.1 mm, 1.7m. Mobile phase containing Buffer: Acetonitrile taken in the ratio 50:50 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was 0.01N KH2PO4(3.0PH)buffer. Temperature was maintained at 30°C. Optimized wavelength selected was 240 nm Retention time of EGZ and SGP were found to be 0.883 min and 1.465 min. %RSD of the EGZ and SGP were and found to be 0.3 and 0.8 respectively. %Recovery was obtained as 99.83% and 100.09% for EGZ and SGP respectively. LOD, LOQ values obtained from regression equations of EGZ and SGP were 0.139, 0.421 and 0.18, 0.56 respectively. Regression equation of EGZ is y = 4300x + 253.6, and y = 6814x + 11844 of SGP. 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

A new simple, accurate, precise and reproducible Reverse Phase-High Performance Liquid Chromatography  method has been developed for the simultaneous estimation of Sitagliptin and Metformin in bulk and pharmaceutical dosage form using Symmetry C18 column (4.6 x 150mm, 3.5mm, Make: XTerra) in isocratic mode. The mobile phase has been prepared by using Potassium Dihydrogen Phosphate and Acetonitrile in different ratio at different pH. Several trials have been performed and it was found that ratio 0f 65:35 of Potassium Dihydrogen Phosphate and Acetonitrile respectively was shown a good peak at pH 5.8 which has been adjusted by using Sodium Hydroxide. The detection was carried out at 254 nm. The method was linear over the concentration range for Sitagliptin 10-30ppl and for Metformin 100-300ppm. The % recoveries of Sitagliptin and Metformin were found to be 99.1 to 100.6% and 98.8 to 100.7% respectively. The validation of method was carried out utilizing International Conference on Harmonization (ICH) guidelines. The described High Performance Liquid Chromatography method was successfully employed for the analysis of pharmaceutical formulations containing combined dosage form.

A new reverse phase high performance liquid chromatography (RP-HPLC) method for the quantitative determination of Sitagliptin in human plasma was developed and validated as per US-FDA guidelines. The drug was spiked in the plasma and extracted with mobile phase by precipitation method. The extracted analyte was injected into an INTERSIL C18 column (150 mm × 4.6 mm, 5μm), maintained at ambient temperature and effluent was monitored at 267 nm. The mobile phase consisting of acetonitrile: methanol: buffer (2:3:5 v/v). The pH of the mobile phase was adjusted to 4.0 by using O-phosphoric acid. The flow rate was maintained at 1.0 mL/min. The developed method shows high specificity for sitagliptin. Calibration curve was plotted with a range from 25-125µg/mL (r2>0.9994). The lower limit of quantification (LLOQ) was found to be 25μg/mL. The method was validated for parameters like accuracy, precision, recovery, linearity, range, stability and sensitivity. This RP-HPLC method is suitable for determining the concentration of sitagliptin in human plasma and it was applied to routine analysis for determination of the Sitagliptin from dosage form during pharmacokinetic study.