J. Pharm. Technol. Res. Manag.

Exploring RP-HPLC Method for analysis of Axitinib in Bulk and in-house Tablets

Shailesh S. Chalikwar, Satish D. Kayande, Inderbir Singh, Atul A. Shirkhedkar

KEYWORDS

Axitinib;HPLC; validation;in-house tablets

PUBLISHED DATE Nov. 2, 2018
PUBLISHER The Author(s) 2018. This article is published with open access at www.chitkara.edu.in/publications.
ABSTRACT

Axitinib is a tyrosine kinase Inhibiter. In a commenced analysis, a effortless and responsive high-performance liquid-chromatography method was developed and validated for the quantitative estimation of Axitinib in bulk and in-house tablet dosage form. The present method was developed and validated using LC-GC Qualisil BDS C18(250 mm × 4.6 mm, 5 µm). The separation of Axitinib was employed using a methanol: water 85:15% v/vas a mobile phase at optimal flow rate 1 mL/min and column oven temperature 30°C. While, Axitinib was examined at 330 nm with a photo diode array detector; retention timewas found to be 3.23 min.The intended method was validated by ICH rules for the accuracy, precision, sensitivity, and ruggedness. The linearity was followed in the concentration range of 4 - 24 µg/mL as demonstrated by correlation coefficient (r2) of 0.9994. The robustness of proposed method was assessed by purposelyvarying the chromatographic conditions.Consequently, the intended method can routinely be subjected for the estimation of Axitinib in bulk and in tablets formulation.

INTRODUCTION

Axitinib is tyrosine kinase Inhibiter and an oral, selective inhibitor of vascular endothelial growth factor receptors 1, 2, and 3 [1,2]. It is a small molecule developed by Pfizer[2]. Axitinib is an indazole derivative, chemically it is N-Methyl-2 [[3-[(e) -2-pyridin-2-ylethyl-1H-indazole-6-yl] sulfanyl]benzamide. The molecular formula of Axitinib is C22H18N4OS and molecular weight is 386.46 gm/mol[3,4]. It specifically restrains vascular endothelial development factor receptors (VEGFR-1, VEGFR-2, VEGFR-3); tumour development and metastases.1,2 Axitinib has been accounted to be 50-450 times more potent than first generation VEGFR inhibitors[5].

In Literature studies, few analytical methods for assessment of Axitinib have been studied, which includes liquid chromatography-mass spectrophotometry (LC-MS/ MS)[6-8], UPLC[9], spectrophotometric[10] and HPLC [3, 11]. To our knowledge, till date no HPLC method has been reported for the assurance of Axitinib in bulk and inhouse tablet dosage form.Therefore, an attempt of proposed work is toestablish a simple, reliable and reproducible RPHPLC method for determination of Axitinib in bulk and in-house tablet dosage form. Also, an established method wasvalidated in accordance with ICH guidelines Q2(B).

Page(s) 135-141
URL http://dspace.chitkara.edu.in/jspui/bitstream/123456789/791/1/JPTRM%206-2-4.pdf
ISSN Print : 2321-2217, Online : 2321-2225
DOI 10.15415/jptrm.2018.62010
CONCLUSION

The proposed developed RP-HPLC method for the estimation of Axitinibin bulk and in-house tablet dosage form using mobile phase composed of methanol: water (85:15 % v/v) showed an admirable separation of Axitinib with retention time was 3.23 min. The established method gives good resolution of Axitinib with short analysis time. The established method was linear over the concentration range of 4-24 µg/ml; with a correlation coefficient (r2) 0.999 along with the obtained LOD and LOQ 0.0199 µg and 0.0602 µgvalues showed the highest sensitivity towards the optimized mobile phase. The method was developed and validated and found to be simple, sensitive, accurate, and precise. Also, the developed methods were compared with the reported methods. Therefore, thedeveloped method can be routinelyused for the analysis of Axitinib in bulk and in- house pharmaceutical dosage form.

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