Development and Validation of a Stability-Indicating High Performance Thin Layer Chromatography (HPTLC) Method for estimation of Canagliflozin in bulk and Pharmaceutical Dosage Form

Abstract

The objective of the study was to develop and validate simple, authentic and stability indicating high performance thin-layer chromatographic method for determination of Canagliflozin in bulk and pharmaceutical formulations as per ICHQ2 R1 Guidelines. HPTLC aluminium plates Precoated with Silica Gel 60F254 using Toluene: Ethyl acetate: Methanol (2:2:1, v/v/v) as mobile phase were used for the chromatographic separation and it was validated with different parameters such as Linearity, Precision, Accuracy, Robustness, Ruggedness, Limit of Detection (LOD) and Limit of Quantification (LOQ). Also, Forced degradation study was carried out in different mediums. The densitometric analysis of the spots was performed at 290 nm. A Linear data over the range of 10-500ng/spot with a good correlation coefficient of 0.9988 unfolds linear relationship between area and concentration in calibration curve. The LOD and LOQ were found to be 0.39 and 1.19 respectively. A recovery of Canagliflozin in tablet formulation was observed in the range of 99.04-99.82%. Percentage assay of Canagliflozin tablets (INVOKANA ® ) was found to be 99.8%. Forced degradation studies of canagliflozin showed the degradation in acidic, alkaline, photolytic and oxidation but were most stable in thermal degradation. The proposed method is definite, meticulous and reproducible and can be used for routine analysis of Canagliflozin in bulk and pharmaceutical dosage form.

Stability‐indicating chromatographic and chemometric methods for environmentally benign determination of canagliflozin and its major degradation product; A comparative study and greenness assessment

“…The main task of this work was to develop and validate eco‐friendly stability‐indicating HPLC and PLS methods for determination of canagliflozin along with its main degradation product as substituents for environmentally harmful reported HPLC methods which did not quantify or even structurally identify the resulting degradation product. The proposed HPLC method can be used as a substitute for the reported TLC–densitometric methods (Kaur, Wakode, & Singh, ; Emam, ) owing to the common advantages of HPLC over TLC–densitometry such as the high repeatability, accuracy, and short analysis time as well. On the other hand, a thorough literature survey showed that there is no reported chemometric method for determination of canagliflozin, making the proposed PLS method the first chemometric one for simultaneous determination of canagliflozin and its degradation product with high specificity and precision.…”

“…A thorough literature survey showed canagliflozin determination by HPLC methods in a pharmacokinetic study ( Devineni et al, ), a pharmaceutical formulation (Kaur, Wakode, Singh, & Manachanda, ) in rat plasma (Iqbal, Ezzeldin, Al‐Rashood, Asiri, & Rezk, ; Iqbal, Khalil, Alanazi, & Al‐Rashood, ; Kobuchi, Yano, Ito, & Sakaeda, ; Dong et al, ), in human plasma (Iqbal, Ezzeldin, et al, ; Iqbal, Khalil, et al, ; Dudhe & Kamble, ; Saibaba, Pilli, Bimireddy, & Pandiyan, ; Udhayavani, Sastry, Rajan, Tejaswi, & Rajani, ), and along with metformin (Gaware, Patil, & Harole, ; Zaghary, Mowaka, & Hendy, ). Canagliflozin was also determined by spectrophotometric (Kaur et al, ; Kaur, Wakode, & Singh, ) and TLC–densitometric methods (Kaur, Wakode, & Singh, ; Emam, ).…”

“…They determined canagliflozin either alone or in combination with other drugs without taking into consideration the environmentally hazardous effects of the chemicals used. Additionally, the reported stability‐indicating assay methods (Gaware et al, ; Kaur, Wakode, & Singh, ) did not pay attention to structural elucidation or quantification of any stress‐degradation product of canagliflozin. Although multivariate calibrations are useful in spectral analysis owing to the simultaneous inclusion of multiple spectral intensities, which greatly improves the precision and the applicability of quantitative spectral analysis (Goicoechea & Olivieri, ; Haaland & Thomas, ; Kramer, ), no chemometric methods have been reported for determination of canagliflozin.…”

Canagliflozin stability study and ecofriendly chromatographic determination of its degradation product: A comparative study

“…The reported HPTLC-densitometric method [11] was based on using toluene which is not environmentally recommended [21] and also used methanol and ethyl acetate which are less preferable than acetone and ethanol from the environmental viewpoint [21].…”

“…In contrast, the proposed HPTLC-densitometric method studied method specificity through structural elucidation, quantification, and chromatographic separation of the degradation product from canagliflozin in one chromatogram in addition to the common advantages of TLC-densitometric methods over the reported HPLC methods [6][7][8][9][10]; being more cost effective and of higher sensitivity. Furthermore in spite of the stability indicating property of the reported TLC-densitometric method, [11] it was able to determine only canagliflozin degraded samples and the degradation was evidenced by the decrease in canagliflozin peak height which is not indicative and according to ICH guidelines [13], peak area must be considered for the change in drug concentration not peak height.…”