Development and validation of a reversed-phase column liquid chromatographic method for simultaneous determination of two novel gliptins in their binary mixtures with Metformin

Mohammad, Mohammad Abdul‐Azim; Elkady, Ehab F.; Fouad, Marwa A.

doi:10.5155/eurjchem.3.2.152-155.570

Cited by 28 publications

(12 citation statements)

References 13 publications

(12 reference statements)

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“…Stability indicating RP HPLC and RP-LC-PDA methods for determination of SAXA in pharmaceutical dosages were developed (Scheeren et al, 2015;Konari, Jacob, 2015). SAXA was estimated, with other antidiabetic drugs like vildagliptin, using spectrophotometric and spectrofluorimetric methods from bulk and pharmaceutical dosage forms (Marwa, 2013) and also with metformin hydrochloride, using the RP column liquid chromatographic method in binary mixtures (Mohammad, Ehab, Marwa, 2012), The HPLC method is used in active drug and pharmaceutical dosage forms (Hanan et al, 2017) and stability indicating RP HPLC method for the determination of saxagliptin and metformin in bulk and pharmaceutical product (Ramesh, Senthil Kumar, 2016). Some analytical procedures have been reported for quantitative determination of DAPA alone by UV spectrophotometry only in API (Manasa et al, 2014) and the RP HPLC method in bulk and tablet dosage forms (Subrata, Vipul, 2017).…”

Section: Introductionmentioning

confidence: 99%

Application of quality by design approach in RP-HPLC method development for simultaneous estimation of saxagliptin and dapagliflozin in tablet dosage form

Gundala

Prasad

Koganti

2019

Braz. J. Pharm. Sci.

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A simple, sensitive, precise, accurate and robust high performance liquid chromatographic method has been developed for simultaneous estimation of saxagliptin (SAXA) and dapagliflozin (DAPA) in pharmaceutical formulation. Design of experiments (DoE) was applied for multivariate optimization of the experimental conditions of RP-HPLC method. Risk assessment was performed to identify the critical method parameters. Three independent factors; mobile phase composition, flow rate and column temperature were used to design mathematical models. Central composite design (CCD) was used to study the response surface methodology and to study in depth the effects of these independent factors. Desirability function was used to simultaneously optimize the retention time and resolution of SAXA and DAPA. The optimized and predicted data from contour diagram consisted of acetonitrile and ortho phosphoric acid (0.1%) in the ratio of 50:50 respectively, at a flow rate of 0.98 ml/min and column temperature 31.4 °C. Using these optimum conditions baseline separation of both drugs with good resolution and run time of less than 6 min were achieved. The optimized assay conditions were validated according to ICH guidelines. Hence, the results clearly showed that Quality by design approach could be successfully applied to optimize RP-HPLC method for simultaneous estimation of SAXA and DAPA.

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Section: Introductionmentioning

confidence: 99%

Application of quality by design approach in RP-HPLC method development for simultaneous estimation of saxagliptin and dapagliflozin in tablet dosage form

Gundala

Prasad

Koganti

2019

Braz. J. Pharm. Sci.

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“…Therefore combination of these drugs in a single tablet is mostly used to achieve best glucose control in blood and for better compliance to therapy [6]. To the best of our knowledge, it is revealed that several reversed-phase high-performance liquid chromatography (RP-HPLC) methods are available for the determination of MTF and VLD ( Figure 1) individually or in combination with other drugs in fixed dose pharmaceutical formulations, while a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is presented for both the drugs in combination [7], but no stability-indicating assay method has been reported [8][9][10]. The present research works to develop a rapid, sensitive, and stability-indicating liquid chromatographic (high-performance liquid chromatography [HPLC]) method for the simultaneous determination of MTF and VLD in tablet and biological samples (human plasma), and the proposed HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines [11].…”

Section: Introductionmentioning

confidence: 99%

Stability-indicating RP-HPLC method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples

Shakoor

Ahmed²,

Ikram

et al. 2020

Acta Chromatographica

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The present work aimed to develop and validate a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples. Isocratic elution of both the analytes was performed at 35 °C by injecting 20 μL into Thermo Hypersil ODS C18 column (5 μm, 4.6 mm× 250 mm), while the flow rate was set to 0.8 mL/min. The mobile phase comprised of methanol, acetonitrile, and phosphate buffer (5:30:65, v/v, pH 3.5), and wavelength was selected at 212 nm. The overall run time per sample was 7.0 min with a retention time of 3.36 and 5.41 min for metformin hydrochloride and vildagliptin, respectively. The calibration curve was linear from 10–140 μg/mL for metformin and 1–14 μg/mL for vildagliptin with a coefficient of determination (R2) ≤ 0.9919, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.13 and 0.97%, respectively. Force degradation studies indicated a complete separation of the analytes in the presence of their degradation products providing a high degree of method specificity. The proposed reversed-phase high-performance liquid chromatography (RP-HPLC) method was demonstrated to be simple and rapid for the determination of metformin hydrochloride and vildagliptin in commercially available tablet and biological samples providing recoveries ranged between 100.13–100.29%.

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“…These methods have included spectrophotometry and spectrouorimetry, 9 HPLC and stability-indicating HPLC methods. 16,[21][22][23][24] However, LC methods based on UV and DAD detectors show moderate sensitivity and selectivity for complex matrices such as plasma. Simultaneous estimation of STG, MET and their impurities was carried out by a stability indicating method manifesting a good separation using HPLC-UV, where STG and MET were estimated in concentration range of 10-150 mg mL À1 and 50-450 mg mL À1 , respectively.…”

Section: Introductionmentioning

confidence: 99%

Novel contribution to the simultaneous analysis of certain hypoglycemic drugs in the presence of their impurities and degradation products utilizing UPLC-MS/MS

Mowaka

Mohamed

2015

RSC Adv.

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A novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of three hypoglycemic drugs namely; sitagliptin (STG), vildagliptin (VLG) and metformin (MET) in the presence of their degradation products and STG related impurities. Chromatographic separation was accomplished on a Hypersil gold 50 mm Â 2.1 mm (1.9 mm) column, using acetonitrile and 0.2% formic acid aqueous solution as the mobile phase with a gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. The selected reaction monitoring (SRM) mode on a triple quadrupole mass spectrometer was used to quantify the drugs utilizing the transitions of 408.12 / 235.24 (m/z), 304.33 / 154.32 (m/z), 130.12 / 71.32 (m/z) and 255.75 / 166.15 (m/z), for STG, VLG, MET and diphenhydramine (IS), respectively. The method has displayed a lower limit of detection of 1.50 ng mL À1 , 1.50 ng mL À1 and 3.00 ng mL À1 for STG, VLG and MET, respectively. The drugs were subjected to forced degradation where it was concluded that STG, VLG and MET were highly susceptible for alkaline stress conditions. In addition, the study of the degradation kinetics of the drugs has proved that the degradation follows a pseudo-first-order reaction.The proposed method was effectively applied for the analysis of laboratory prepared mixtures as well as combined pharmaceutical formulations. No significant difference was found regarding accuracy and precision upon statistical comparison of the obtained results with those of the reported method.Validation was conducted in compliance with the ICH guidelines proving the method to be selective, linear, precise and accurate. The simplicity and sensitivity of this method allows its use in the quality control of the cited drugs. Scheme 1 The proposed structures and pathways of the main degradation products of STG produced under (a) alkaline degradation and (b) acid degradation. 60476 | RSC Adv., 2015, 5, 60467-60481 This journal is

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Development and validation of a reversed-phase column liquid chromatographic method for simultaneous determination of two novel gliptins in their binary mixtures with Metformin

Cited by 28 publications

References 13 publications

Application of quality by design approach in RP-HPLC method development for simultaneous estimation of saxagliptin and dapagliflozin in tablet dosage form

Application of quality by design approach in RP-HPLC method development for simultaneous estimation of saxagliptin and dapagliflozin in tablet dosage form

Stability-indicating RP-HPLC method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples

Novel contribution to the simultaneous analysis of certain hypoglycemic drugs in the presence of their impurities and degradation products utilizing UPLC-MS/MS

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