AUTHENTICATION OF BOTANICALS AND HERBAL PRODUCTS USING UPLC/ION MOBILITY QTOF-MS AND A METABOLOMICS APPROACH

Importance of the topic

Monitoring authenticity of herbal products addresses safety, efficacy and consumer trust. Fadogia agrestis supplements have recognized therapeutic uses but face significant adulteration risks. High-resolution metabolomics with UPLC-IMS-QTof-MS provides detailed chemical fingerprints to detect substitutions and ensure product integrity.

Objectives and Study Overview

• Identify key metabolites differentiating authentic Fadogia agrestis from commercial products
• Develop a multi-marker metabolite database for routine authentication using nominal mass instruments

Methodology and Instrumentation

Sample preparation involved methanol extraction of 10 reference specimens and 17 commercial formulations with repeated vortexing and centrifugation. A pooled QC sample ensured analytical robustness.

• Chromatography: ACQUITY UPLC I-Class FTN with HSS T3 1.8 μm column, water and acetonitrile with 0.1 FA, flow rate 0.5 mL/min, 40 °C, injection 1 μL
• Mass spectrometry: Waters Vion IMS QTof, high-definition MSE in positive and negative ESI, mass range 100–1200 Da, low and high collision energies
• Data analysis: Progenesis QI for alignment, peak picking, compound identification, and multivariate statistics; randomized triplicate injections per sample

Main Results and Discussion

PCA of negative ion data placed all reference samples within a 95 confidence interval around the QC center. Fourteen of seventeen commercial products clustered with authentic material. Loadings plots highlighted significant features distinguishing the groups. One marker at 14.63 min (m/z 920.4563) was confirmed by exact mass, isotope pattern and in silico fragmentation matching. A panel of robust chemical markers was established for authentication.

Benefits and Practical Applications

• Rapid non-targeted metabolomic fingerprinting without reliance on a single analyte
• Enhanced detection of adulteration and substitution in botanical supplements
• Adaptable workflow for routine quality control using both high-resolution and nominal mass instrumentation

Future Trends and Applications

Advances in ion mobility separation for isomer resolution, expansion of marker libraries to additional botanicals, and integration of machine learning for automated classification will strengthen authentication workflows. Standardized metabolomics databases will support regulatory compliance and consumer confidence.

Conclusion

A structured UPLC-IMS-QTof-MS metabolomics workflow combined with multivariate analysis enables reliable authentication of Fadogia agrestis. The multi-marker panel established here provides a foundation for routine quality control and protection against herbal product adulteration.

References

1. Yakubu et al Evaluation of biochemical indices and testicular histology in rats following Fadogia agrestis extract African Journal of Biochemistry 2007 1 156-163