Development and Validation of a Novel RP-HPLC Analytical Method for Sitagliptin Determination in Human Plasma (original) (raw)
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LATIN AMERICAN JOURNAL OF PHARMACY
. Sitagliptin is a new oral selective DPP4 inhibitor anti-diabetic drug. The objective of this study was to develop and validate a new HPLC method for the quantification of sitagliptin and its application in spiked plasma and tablet dosage form. The method was developed by using the C 18 ODS Hypersil column of 150 × 4.6 mm id with 5 μm particle size, mobile phase of acetonitrile and 0.01N potassium dihy-drogen phosphate (70:30) at a flow rate of 1.0 mL/min. Eluate was detected at 269 nm with the retention time of 5.6 min. The limit of detection and limit of quantification were 0.095 and 0.19 μg/mL, respectively. Loratidine was used as an internal standard that co-eluted at 8.3 min. The method was found linear in the range of 0.19-200 μg/mL and %CV was within limits of FDA guidelines. The calibration curve was linear with the equation y = 1.9308x + 7.5227 with a correlation coefficient of 0.999. Accuracy of percentage recovery for between-batches and within batch assays was 97.79-101...
Analytical Methods for Determination of Sitagliptin : An Updated
2017
Sitagliptin is an oral anti-hyperglycemic agent of the dipeptidyl peptidase-4 (DPP-4) inhibitor class used in the treatment of type-2 diabetes. It stimulates insulin release and reduces glucagon level by inhibition of inactivation of the incretin in a glucose-dependant manner. In 2013 it was the second best-selling drug in the U.S. This review explores the reported analytical methods so far in the literature for the estimation of sitagliptin in bulk drug, pharmaceutical formulations and in biological matrix. This assessment encompasses various analytical methods such as spectrometry, high performance liquid chromatography (HPLC), liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS-MS), liquid chromatography-mass spectrometry (LC-MS), capillary electrophoresis (CE), ultra performance liquid chromatography (UPLC), high performance thin layer chromatography (HPTLC) and gas chromatography-mass spectrometry (GC-MS) for the estimation of sitagliptin in single and/or...
2015
International Journal of Pharmaceutical Sciences Review and Research Available online at www.globalresearchonline.net © Copyright protected. Unauthorised republication, reproduction, distribution, dissemination and copying of this document in whole or in part is strictly prohibited. © Copyright protected. Unauthorised republication, reproduction, distribution, 194 Mohamed Karam Qassas, Mohammad Ameral-mardini, Heba Ghazal Faculty of Pharmacy, University of Damascus, Syria. Dept. of Pharmaceutical Chemistry and Quality control, Faculty of Pharmacy, University of Damascus, Syria. PhD Dept. of Pharmaceutical Chemistry and Quality control, Faculty of Pharmacy, University of Damascus, Syria. Heba Ghazal, School of Pharmacy and Chemistry, Kingston University, London, United Kingdom. *Corresponding author’s E-mail: karamqassas@hotmail.com
Indian Research Journal of Pharmacy and Science, 2019
A novel, simple and economic reverse phase high performance liquid chromatographic method was developed and validated as per the ICH guidelines for the quantitative estimation of Sitagliptin Phosphate in pharmaceutical tablet dosage form with greater precision and Accurac Orthophosphoric acid (40:55:5). The eluent was monitored at 265 nm, at a flow rate of 1 mL/min and retention time was observed at 10 min. calibration curve as linear over the concentration range of 6 determination of precision was <2%. Accuracy of method was determined through recovery studies which were found to be 99.82-101.87%. The LOD and LOQ were found to be 0.05 mg/mL and 0.16 mg/mL respectively. Validation studies demonstrated that the proposed RP reproducible. Hence the proposed method can be applied for the routine quality control analysis of Sitagliptin Phosphate in bulk and Pharmaceutical tablet dosage forms.
A simple, rapid, accurate, precise and novel high-performance liquid chromatographic method for simultaneous analysis of Sitagliptin (SITA) and Simvastation (SIMV) in pharmaceutical dosage form has been developed and validated. The chromatographic separation was accomplished on Welchrom RP-C 18 Column (250 mm X 4.6 mm; 5µm), Shimadzu LC-20AT Prominence Liquid Chromatograph and with a mixture of 10 mM Phosphate buffer: acetonitrile and methanol in the range of (45:35:20 v/v/v). The flow rate was fixed at 1mL/minute and the analysis was performed using Shimadzu SPD-20A Prominence UV-detection was performed at 255 nm. The SITA and SIMV were separated within seven minutes. The retention time for SITA and SIMV was found to be 3.352 minutes and 5.402 minutes respectively. The calibration plots were linear over the concentration range of 10-50 µg/ml for SITA (r 2 = 0.9998) and 4-20 µg/ml for SIMV (r 2 = 0.9999). There was no interference due to commonly used excipients. The relative standard deviation for inter-day precision was lower than 2.0 % which obviously indicates that the present method was said to be highly precise. Regarding accuracy of the developed method the % RSD were also found less than 2 % which shows the method is completely accurate. The method was very sensitive with regard to LOD 0.681 µg/ml, 0.116 µg/ml and LOQ 2.250 µg/ml, 0.384 µg/ml respectively. The mean assay values for SITA and SIMV were determined in tablet dosage form were found to be within limits. The developed RP HPLC method was found to be simple, rapid, sensitive, highly precise and accurate highly suitable for routine analysis of drug samples containing SITA and SIMV.
2013
A few methods are available for routine analysis of sitagliptinphosphate and metformin hydrochloride. Here we have developed a simple, precise and stability-indicating HPLC method and validated for the simultaneous determination of sitagliptinphosphate and metformin hydrochloride in pharmaceutical dosage form.The method involves the use of easily available inexpensive laboratory reagents. The method was carried out on a Supelco Column (25cm×4.6mm i.d; particle size 5-microns) with a mobile phase consisting of (70:30 v/v Acetonitrile: ammonium acetate buffer) at a flow rate of 0.8 ml/min.The retention time of the sitagliptin and metformin was about 6.54 and 4.24mins respectively. The method was validated for specificity, linearity, precision, accuracy, robustness and solution stability. The described method was linear over a concentration range of 10-50 μg/ml and 1-5 μg/ml for the assay of metformin and sitagliptin respectivelywith a correlation coefficient of 0.999.The accuracy (rec...
Dhaka University Journal of Pharmaceutical Sciences
A novel reversed phase ultra-high performance liquid chromatographic (RP-UHPLC) method was developed for the estimation of sitagliptin in pharmaceutical dosage form. Separation was done by a X-bridge C18 column (4.6 i.d.× 150 mm, 5 μm particle size) with a flow rate of 1 ml/min using phosphate buffer (pH 6) and acetonitrile (70:30, v/v) as mobile phase at 268 nm using photodiode array plus (PDA+) detector. The retention time was found at 4.607 min. The developed method was validated as per the requirements of ICH-Q2B guidelines for specificity, system suitability, linearity, precision, accuracy, sensitivity and robustness. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.999 with LOD value of 0.06 μg/ml and LOQ of 0.225 μg/ml. The relative standard deviation (%RSD) for inter-day and intra- day precision was not more than 2.0%. The method was found to be accurate with percentages recovery of 98.50±0.03 to 99.70±0.05 and the % RSD w...
Indian Journal of Pharmaceutical Sciences
A new stability-indicating high-performance liquid chromatographic method for simultaneous analysis of sitagliptin and simvastatin in pharmaceutical dosage form was developed and validated. The mobile phase consisted of methanol and water (70:30, v/v) with 0.2 % of n-heptane sulfonic acid adjusted to pH 3.0 with ortho phosphoric acid was used. Retentions of sitagliptin and simvastatin were 4.3 min and 30.4 min, respectively with a flow rate of 1 ml/min on C8 (Qualisil BDS, 250×4.6 mm, 5 μ). Eluents were detected at 253 nm using photodiode diode array detector. The linear regression analysis data for the linearity plot showed correlation coefficient values of 0.9998 and 0.9993 for sitagliptin and simvastatin, with respective concentration ranges of 20-150 μg/ml and 8-60 μg/ml. The relative standard deviation for inter-day precision was lower than 2.0%. The assay of sitagliptin and simvastatin was determined in tablet dosage form was found to be within limits. Both drugs were subjected to a variety of stress conditions such as acidic, basic, oxidation, photolytic, neutral and thermal stress in order to achieve adequate degradation. Results revealed that considerable degradation was found in all stress conditions except oxidative degradations. The method has proven specificity for stability indicating assay method.
Development and Validation of New Spectrophototmetric Methods for the Determination of Sitagliptin
Acta Scientific Pharmaceutical Sciences, 2020
Sitagliptin (Figure 1) is an antidiabetic agent which is an oral dipeptidyl peptidase-4 inhibitor which exerts its actions in type 2 diabetes patients by slowing the inactivation of incretin hormones. Sitagliptin (C 16 H 15 F 6 N 5 O; Mol. Wt. 407.314 g/mol) is chemically (R)-4-oxo-4-[3-(trifluoromethyl)-5,6-dihydro [1,2,4] triazolo [4,3a] pyrazin-7(8H)-yl]-1-(2,4,5-Trifluoro phenyl) butan-2 amine. It stimulates insulin secretion when hyperglycemia is present and inhibits glucagon secretion [1-4]. Various spectrophotometric methods [5-19] have been developed for the assay of Sitagliptin in literature and the present methods were compared with the previously published methods. The authors have chosen five different reagents for the assay of Sitagliptin in pharmaceutical dosage forms present study and validated [20].
International Journal of Experimental Research and Review, 2023
To treat type 2 diabetes, in a combined tablet dosage form the ertugliflozin and sitagliptin were administered. Considering the less complication and readily availability of HPLC, the main objective of present study was to develop a new, precise, accurate, linear, robust, and economical RP-HPLC method for the simultaneous estimation of ertugliflozin and sitagliptin in tablet dosage form. Effective chromatographic separation of Ertugliflozin and Sitagliptin was achieved on Kromasil C18 (5 µm 250 mm X 4.6 mm) and the mobile phase containing Methanol and 0.1% OPA in water isocratic elution mode at a flow rate of 1.0mL/min. with column temperature at 30 °C and the injection volume was 20 µL at column temperature at 30°C. At an isosbestic wavelength of 212 nm, ertugliflozin and sitagliptin were found to have retention times of 5.30 min. and 2.05 min., respectively. The method was proven to be precise (%RSD 2%), accurate (>90%), and specific for the simultaneous measurement of both drugs in tablets. As a result, the suggested method with excellent specificity, accuracy, precision, linearity and robustness as well as economical was useful for the regular quality control analysis of ertugliflozin and sitagliptin tablets.