Development and Validation of a LC-ESI-MS/MS Based Bioanalytical Method for Dapagliflozin and Saxagliptin in Human Plasma

Goday, Swapna; Shaik, Abdul Rahaman; Avula, Prameelarani

doi:10.5530/ijper.52.4s.108

Cited by 16 publications

(6 citation statements)

References 5 publications

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“…The polynomial equation revealing percent extraction recovery, R1 for MET was +70. Validation of bioanalytical method was carried out [25] . For both the drugs, linearity was obtained in the range of 0.022-2.2 μg/ml for MET and 0.0012-0.12 μg/ml for ALO with correlation coefficient of 0.9907 and 0.9918 respectively (Table 2).…”

Section: Resultsmentioning

confidence: 99%

Box-Behnken Design Assisted Protein Precipitation Optimization for Simultaneous Determination of Metformin Hydrochloride and Alogliptin Benzoate in Plasma along with Pharmacokinetic Application

Patel¹,

Patel²,

Shah³

et al. 2021

ijps

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Patel et al.: Simultaneous Determination of Metformin Hydrochloride and Alogliptin Benzoate in PlasmaThe study focuses on systematic quality by design oriented approach for the optimization of a sensitive reverse phase liquid chromatographic bioanalytical method for determination of metformin hydrochloride and alogliptin benzoate in plasma along with its validation. Chromatographic separation was carried out on C 18 column using gradient mode with mobile phase; 1-octane sulphonic acid (10 mM), acetonitrile and phosphate buffer pH 4, adjusted by orthophosphoric acid, at 1.0 ml/min using 235 nm as detection wavelength. A Box-Behnken design was applied to protein precipitation sample extraction method with centrifugation speed, centrifugation time and volume of plasma as the critical method parameters for maximizing percentage extraction recovery of metformin hydrochloride and alogliptin benzoate as the critical analytical attributes. The optimized condition for centrifugation speed, centrifugation time and volume of plasma considered as the critical method parameters for maximizing extraction recovery were 11 800 rpm, 15 min, 100 μl. This optimized extraction method gave clear samples and resulted in good correlation in the concentration range of 0.022-2.2 and 0.0012-0.12 μg/ml for metformin hydrochloride and alogliptin benzoate, respectively. The mean percentage extraction recoveries at three quality control levels were 90.83-95.87 % for metformin hydrochloride and 94.03-96.73 % for alogliptin benzoate. The plasma concentration time profile showed higher peak plasma concentration for formulation compared to pure drugs indicating that absorption of metformin and alogliptin hydrochloride from formulation was better. The developed liquid chromatographic method presented good quantitative capability, good linearity, higher extraction recovery, simpler operation and short analysis time with low cost.

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Section: Resultsmentioning

confidence: 99%

Box-Behnken Design Assisted Protein Precipitation Optimization for Simultaneous Determination of Metformin Hydrochloride and Alogliptin Benzoate in Plasma along with Pharmacokinetic Application

Patel¹,

Patel²,

Shah³

et al. 2021

ijps

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“…Literature review shows minimal methods has been developed and reported for Dapagliflozin estimation by HPLC as an individual drug [3,[17][18][19][20] and in combination with Saxagliptin and Metformin [21][22][23][24] where the reported methods has vary retention time, high run time and more consumption of organic solvents for the estimation. This study focused on developing an RP-HPLC method of Dapagliflozin which is more economical, new, rapid, precise and accurate with a good amount of separation, consuming less organic solvents for separation as compared to the reported research work mentioned above.…”

Section: Fig 1: Chemical Structure Of Dapagliflozinmentioning

confidence: 99%

Simple Quantified and Validated Stability Indicating Stress Degradation Studies of Oral Anti-Diabetic Agent Dapagliflozin by Rp-HPLC Method

Murugesan¹,

Annapurna

2022

Int J App Pharm

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Objective: This method is focused on developing a precisely simplified and more accurate Reverse Phase–High Pressure Liquid Chromatography (RP-HPLC) method for the determination of Dapagliflozin in bulk and pharmaceutical dosage form as per guidelines of International Council for Harmonization (ICH). Methods: Evaluation and validation carried out using the RP-HPLC ZORBAX (C18) column (250 x 4.6 mm, 5 μm particle size) with a mobile phase consisting of Phosphate Buffer: Acetonitrile: Methanol in a ratio of 55:40:05 (v/v/v) at a flow rate of 1 ml/min with an injection volume of 10 μl. Results: Dapagliflozin was eluted at 2.12±0.05 min and detected at 225 nm. The regression equation y = 55762 x-29679 found to be linear with correlation coefficient r2 value of 0.9997. The developed RP-HPLC method was conveniently validated as per the ICH guidelines and found method was robust, sensitive, accurate, selective, specific, precise and linear. Conclusion: The proposed method was found to be accurate, precise, and robust for API and pharmaceutical dosage form as per experimentation analysis. The above developed method was found to be satisfied for Active Pharmaceutical Ingredient (API) and pharmaceutical formulation of Dapagliflozin to study its degradation products.

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“…Now a day, stability indicating method as important regulatory and CGMP point of view to assess the drug stability. In the present study, it was tired to develop stability indicating RP-HPLC method to determine possible degradation products of DAPA and MET [18][19][20][21][22][23][24][25].…”

Section: Introductionmentioning

confidence: 99%

Stability Indicating HPLC Method Development and Validation for Simultaneous Estimation of Dapagliflozin and Metformin Tablet Dosage Form

NANDRE¹,

AHMED²,

GJ³

2022

Asian J Pharm Clin Res

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Objectives: The objective of this study was to developed and validated for the routine analysis of dapagliflozin (DAPA) and metformin (MET) in API and tablet dosage forms. Methods: The estimation of DAPA and MET was accomplished with C18 column (4.6 × 250 mm and 5 μm particle size) with DAD detector. The mobile phase consists of Methanol: Water 75:25% v/v of pH-3 adjusted with 0.05% OPA at flow rate of 1 mL/min. The detection wavelength was 233nm, respectively. Results: In the developed method, the retention time of DAPA and MET was found to be 5.099 min and 2.165 min. The reverse phase high performance liquid chromatography method produces linear response that were found in the range of 100–500 μg/mL. The limit of detection and limit of quantification for DAPA were found to be 0.06 μg/mL and 0.1855 μg/mL, respectively and for MET 6.09 μg/mL and 18.45 μg/mL, respectively. Calculated information acquired for both the preliminaries roughly coordinates with the information given by design expert programming which shows the genuineness of the chromatographic condition. Conclusion: The developed method was validated according to the ICH guidelines. The linearity, precision, range, and robustness were within the limits as specified by the ICH guidelines. Hence, the method was found to be simple, accurate, precise, economic, and reproducible.

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Development and Validation of a LC-ESI-MS/MS Based Bioanalytical Method for Dapagliflozin and Saxagliptin in Human Plasma

Cited by 16 publications

References 5 publications

Box-Behnken Design Assisted Protein Precipitation Optimization for Simultaneous Determination of Metformin Hydrochloride and Alogliptin Benzoate in Plasma along with Pharmacokinetic Application

Box-Behnken Design Assisted Protein Precipitation Optimization for Simultaneous Determination of Metformin Hydrochloride and Alogliptin Benzoate in Plasma along with Pharmacokinetic Application

Simple Quantified and Validated Stability Indicating Stress Degradation Studies of Oral Anti-Diabetic Agent Dapagliflozin by Rp-HPLC Method

Stability Indicating HPLC Method Development and Validation for Simultaneous Estimation of Dapagliflozin and Metformin Tablet Dosage Form

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