Development of quantitative HPTLC-densitometry methods following a model process for transfer of TLC screening methods for pharmaceutical products containing moxifloxacin HCl, ofloxacin, amoxicillin trihydrate, acetylsalicylic acid + acetaminophen + caffeine, nimesulide, irbesartan, and pantoprazole

Abstract

Transfer of thin-layer chromatography (TLC) Global Pharma Health Fund E.V. Minilab Manual and U.S. Food and Drug Administration (FDA) Compendium protocols for detecting falsified or substandard drugs in pharmaceutical products to quantitative high-performance TLC (HPTLC)-densitometry methods suitable for support of regulatory authorities was performed following a previously published model process for moxfloxacin HCl, ofloxacin, and amoxicillin trihydrate. In addition, the guidelines of the process were followed to develop and validate HPTLC-densitometry methods for pharmaceutical products containing acetylsalicylic acid + acetaminophen + caffeine, nimesulide, irbesartan, and pantoprazole that are not included in the Minilab Manual or FDA Compendium. The new methods involved silica gel 60 F₂₅₄ plates; semiautomated bandwise sample and standard solution application; ascending mobile phase development of plates in a glass chamber; and automated slit scanning densitometry for detection, identification, and quantification. Data for standard and sample solution preparation, calibration curves, assay of pharmaceutical products compared to label declarations, standard addition validation, and peak purity and peak identity are provided. Supplemental FDA Compendium screening methods corresponding to the HPTLC-densitometry methods for caffeine, nimesulide, irbesartan, pantoprazole, and acetylsalicylic acid co-formulated with acetaminophen and caffeine were developed and published online with open access on the website www.layloff.net.

Graphical Abstract

Keywords:

• Thin layer chromatography; substandard drugs; counterfeit drugs; Minilab; transfer of TLC drug screening methods to HPTLC densitometry; FDA compendium

Acknowledgements

We thank Professor Eliagiringa Kaale, School of Pharmacy, Muhimbili University of Health and Allied Sciences, Dar es Saleem, Tanzania, for arranging delivery of drug product samples. We thank Dr. Gerd Battermann, Head of Instrumental Analytics Franchise, Merck KGaA, Darmstadt, Germany, for providing the HPTLC plates used in our experiments. Ellen Armor performed research that led to discovery of the mobile phase used for the successful analysis of amoxicillin. Kaitlin Nguyen’s research was carried out in the Independent Research course required for her graduation from Lafayette College with a B.S. degree in Biochemistry.

Additional information

Funding

Bingsong Zeng was financially supported by a Larkin Professional Development Fund awarded to Professor Sherma and Yiru Gu by the Lafayette College EXCEL Scholars Program.