An HP-TLC densitometric method and fingerprinting for estimating capecitabine and thymoquinone simultaneously and its application in nanoscience using Box–Behnken design

Abstract

World Health Organization estimates that 10% of medications are of inferior quality, thus dangerous to human health. One way to avoid such a problem is to create an adequate, economical, and competitive analytical system. As a result, the study’s goal is to create a High-Performance Thin Layer Chromatography (HP-TLC) method for determining capecitabine (CAP) and thymoquinone (TQ) simultaneously. To the best of our knowledge, no such method for determining CAP and TQ simultaneously exists today. The method was created by implementing an analytical quality-by-design approach based on the Box–Behnken design (BBD) to optimize the chromatographic conditions and a combination of factors such as toluene volume (A), solvent front (B), and chamber saturation time (C), all of which were likely to affect the R_f of CAP and TQ, respectively, later validated using TLC-silica coated plate 60 F₂₅₄. The validated parameters were within an acceptable range, according to ICH guidelines. BBD design revealed that the volume of toluene and solvent front had a greater effect on all of the responses studied and thus needs to be controlled. The developed method of the analysis was found to be facile, dependable, expeditious, cost-effective, and could be used to quantify CAP and TQ in Nanoformulation.

Graphical Abstract

RESEARCH HIGHLIGHTS

• To determine both the drugs in nanoformulation, an accelerated and expeditious densiometric HP-TLC method was developed and validated.

• Particle size, zeta potential, entrapment efficiency (EE), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) analysis were all performed on the prepared nanoformulation.

• According to ICH guidelines, the developed method has been tested for linearity, range, detection limit, quantification limit, precision, and robustness.

• A review of the literature reveals that there are several methods for determining CAP and TQ individually but no HP-TLC method has been reported for simultaneous estimation of CAP and TQ in the combined dosage form.

• Changes in mobile phase volume and changes in chamber saturation duration showed percent RSD-within the 2% criterion, confirming the robustness of the developed method.

Keywords:

• Box–Behnken design
• capecitabine
• densitometry
• HP-TLC
• nanoformulation
• thymoquinone

Acknowledgments

The authors would also like to thank the director of the Analytical Laboratory at KAHER's BSRC in Belagavi, Karnataka, India, for providing the facilities needed to complete this study.

Disclosure statement

No potential conflict of interest was reported by the author(s).