Title:Analytical Method Development, Validation and Forced Degradation
Study of Dapagliflozin by RP-HPLC
Volume: 16
Issue: 2
Author(s): Ujwal Chaudhari, Jagdish K. Sahu*Payal R. Dande
Affiliation:
- School of Pharmacy & Technology Management, SVKM’s NMIMS (Deemed to be University), Shirpur, Distt - Dhule (Maharashtra), 425405, India
Keywords:
Dapagliflozin, RP-HPLC, degradation, analytical validation, ICH guideline, T2DM.
Abstract:
Background: Worldwide, it is projected that 285 million individuals have diabetes, and
by 2030, this number is expected to climb to 438 million. About 90% of cases of diabetes mellitus
are type 2 (T2DM). Insulin sensitizers, such as metformin and thiazolidinediones; insulin secretagogues,
such as sulfonylureas and glinides; dipeptidyl peptidase 4 (DPP-4) inhibitors; glucosidase
inhibitors, or oral combination therapy are currently available treatments for type 2 diabetes.
Some of these drugs exhibit serious limitations; thus, it is crucial to design an innovative therapy
that is efficient and depends on a new channel.
Aim: In the current work, a stability-indicating reverse phase HPLC (RP-HPLC) technique was
developed and subsequently validated for the detection of dapagliflozin in its API.
Methods: The stability-indicating HPLC method for assay included the use of Kromasil 100-5-C8
(100 mm × 4.6 mm) column, UV detector 224 nm, mobile phase composition involving a mixture
of acetonitrile:water (52:48), and a flow rate of 1.0 mL/min. ICH guidelines were followed for the
method's validation. To assess the method's specificity and stability in showing characteristics,
stress degradation studies were carried out. The working standard solution of dapagliflozin was
exposed to 1 and 2 N HCl by refluxing 1 and 2 N NaOH with 30% hydrogen peroxide by volume
and UV radiation in order to conduct a degradation study.
Results: All system suitability parameters were determined to be within the intended ranges, and
the drug's retention duration was discovered to be 1.67 minutes. It was also investigated as to how
the drug degraded under various circumstances. The drug was discovered to be stable under situations
of photolytic, thermal, neutral, alkaline, and oxidative deterioration. The developed stabilityindicating
HPLC technique was validated in accordance with ICH Q2 recommendations, and the
validation parameters, such as linearity, precision, and robustness, were achieved within the approved
standards.
Conclusion: It may be concluded that this method is stability-indicating and specific, and it can
be successfully applied to analyze tablet dosage forms containing dapagliflozin.