SIMPLE QUANTIFIED AND VALIDATED STABILITY INDICATING STRESS DEGRADATION
STUDIES OF ORAL ANTI-DIABETIC AGENT DAPAGLIFLOZIN BY RP-HPLC METHOD
Original Article
ARULSELVAN MURUGESAN
1*
, MUKTHINUTHALAPATI MATHRUSRI ANNAPURNA
2
1
Department of Pharmaceutical Analysis, AIKTC School of Pharmacy, New Panvel 410206 Dist-Raigad (M. S.) India,
2
Department of
Pharmaceutical Analysis and Quality Assurance, GITAM Institute of Pharmacy, GITAM (Deemed to be University), Visakhapatnam 530045,
India
*
Email: arulrama@gmail.com
Received: 29 Oct 2021, Revised and Accepted: 08 Dec 2021
ABSTRACT
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 r
2
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.
Keywords: Dapagliflozin, Forced stability, ICH, SGLT2, Stress degradation, RP-HPLC, Validation
© 2022 The Authors. Published by Innovare Academic Sciences Pvt Ltd. This is an open access article under the CC BY license (https://creativecommons.org/licenses/by/4.0/)
DOI: https://dx.doi.org/10.22159/ijap.2022v14i1.43482. Journal homepage: https://innovareacademics.in/journals/index.php/ijap
INTRODUCTION
Dapagliflozin (C21H25ClO6) is chemically namedas (1S)-1, 5-anhydro-
1-C-[4-chloro-3-[(4-ethoxyphenyl) methyl] phenyl]-D-glucitol,
physical appearance of it is a white to off white solid with melting
range of 74-78 °C. The molecular weight is 408.873 g/mol. It has a
good solubility profile in organic solvents such as methanol, and
dimethyl sulfoxide but is poorly soluble in aqueous media.
Fig. 1: Chemical structure of dapagliflozin
Dapagliflozin is an oral anti-diabetic agent which belongs to
Selective Sodium-glucose co-transporter-2 (SGLT2) Inhibitor.
Sodium-glucose co-transporter-2 (SGLT2) inhibitors are expressed
in proximal renal tubules and are responsible for 90% reabsorption
of glucose filtered by kidneys. Sodium-glucose co-transporter 2
(SGLT2) lowers reabsorption of filtered glucose into the body by
decreasing the renal threshold for glucose (RTG) which leads to the
production of a supplement to urinary glucose excretion in diabetic
patients [1, 2]. Dapagliflozin is a C-glycosyl comprising beta-D-
glucose in which the anomeric hydroxyl group is replaced by a 4-
chloro-3-(4-ethoxybenzyl) phenyl group to improve glycemic
control in adults with type 2 diabetes along with improved lifestyle.
Adults with proper diet and exercise showed improved glycemic
control by Gliflozin derivatives by inhibiting glucose resorption in
the proximal tubule of the nephron and causing glycosuria [2, 3].
Various studies performed and reported for estimation of gliflozin
derivatives and Dapagliflozin using Ultraviolet-Visible (UV-Vis)
spectroscopy as single dosage form [4-6] as well as in its
combination form [7-10].
Few researchers studied its pharmacokinetics in biological fluids by
selecting Bioanalytical methods [11-13] and there are some other
methods reported like HPTLC, Fluorescence and capillary
electrophoresis for estimation of Dapagliflozin, in combination with
other anti-diabetic agents like Saxagliptin/Metformin [14-16].
Literature review shows minimal methods has been developed and
reported for Dapagliflozin estimation by HPLC as an individual drug
[3, 17-20] and in combination with Saxagliptin and Metformin [21-
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.
MATERIALS AND METHODS
Chemicals and reagent
For this study, HPLC grade Acetonitrile (ACN), HPLC grade Methanol
(MeOH), HPLC grade O-Phosphoric acid (OPA) from Merck (Mumbai,
India) and HPLC grade water of SD fine-Chem Ltd; Mumbai were
utilized. Market samples of FORXIGA 10 mg tablets of Dapagliflozin
were purchased from a local chemist shop.
Instrumentation and optimized chromatographic conditions
Shimadzu 2010CHT HPLC system supplied with a gradient pump
connected to a UV detector set at 225 nm used. Lab solution software
(5.5.2 Version) was used for data acquisition and for system suitability
International Journal of Applied Pharmaceutics
ISSN- 0975-7058 Vol 14, Issue 1, 2022