Stability indicating HPTLC method development and validation for the analysis of novel nitroimidazole antitubercular drug delamanid

Abstract

Background and Aims: Delamanid is an active drug substance used in efficient treatment for multidrug-resistant tuberculosis (MDR TB). A straightforward, accurate, and precise HPTLC technique has been developed and validated for the study of the delamanid. Methods: The samples were placed as bands on an aluminium TLC plate covered with silica gel. Delamanid was completely separated using ethyl acetate and n-hexane as the mobile phase; the RF value was 0.51 0.098. At 330 nm, densitometric detection was performed in the absorbance mode. This method led to the discovery of sharp, symmetrical, and well-defined peaks. Results: A linear correlation was obtained for the concentration range of 200–1200 ng/spot, with a determination coefficient of 0.992. According to the requirements set out by the International Conference on Harmonisation, the method’s accuracy, recovery, repeatability, and robustness were all validated. The limit of quantitation was determined to be 349.11 ng/spot, whereas the lowest detectable level was found to be 115.2 ng/spot. This approach permitted the analysis of delamanid in the presence of their degradation products created under various stress conditions, according to the findings of the validation research. delamanid degraded by 20.54% and 35.72% under alkaline and photodegradation conditions, respectively. Conclusion: The established method might be used to evaluate the stability of delamanid in a commercial pharmaceutical dose form. Regarding HPTLC-induced degradation of delamanid, no prior technique has been documented. This technique was successfully used to quantify the amount of delamanid in its commercially available formulation.

Keywords

• HPTLC
• Method Development
• Validation
• Stability indicating method
• Delamanid

References

1. Bahuguna, A., & Rawat, D. S. (2020). An overview of new antituber-cular drugs, drug candidates, and their targets. Medicinal research reviews, 4 0(1), 263-292. google scholar
2. Ferenczi-Fodor, K., Renger, B., & Vegh, Z. (2010). The frustrated reviewer—recurrent failures in manuscripts describing validation of quantitative TLC/HPTLC procedures for analysis of pharma-ceuticals. JPC-Journal of Planar Chromatography-Modern TLC, 23(3), 173-179. google scholar
3. Field, S. K. (2013). Safety and efficacy of delamanid in the treatment of multidrug-resistant tuberculosis (MDR-TB). Clinical Medicine Insights: Therapeutics, 5, CMT-S11675. google scholar
4. Guideline, I. H. T. (1996). Stability testing: photostability testing of new drug substances and products. Q1B, Current Step, 4. google scholar
5. ICH, I. C. H. (2005). Topic Q2 (R1) validation of analytical Proce-dures: text and methodology. In Int. Conf. Harmon (Vol. 1994, p. 17). google scholar
6. Le Roux, A. M., Wium, C. A., Joubert, J. R., & Van Jaarsveld, P. P. (1992). Evaluation of a high-performance thin-layer chromato-graphic technique for the determination of salbutamol serum lev-els in clinical trials. Journal of Chromatography B: Biomedical Sciences and Applications, 581(2), 306-309 google scholar