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Planta Med 2023; 89(09): 860-878
DOI: 10.1055/a-2002-2260
Biological and Pharmacological Activity
Original Papers

Development of an Analytical Workflow to Support the Establishment of Monographs in African Pharmacopoeias – Combretum mucronatum Leaves as Example

Emmanuel Orman
1   Institute of Pharmaceutical Biology and Phytochemistry, University of Münster, Münster, Germany
2   Department of Pharmaceutical Chemistry, School of Pharmacy, University of Health and Allied Sciences, Ho, Ghana
3   Department of Pharmaceutical Chemistry, Faculty of Pharmacy and Pharmaceutical Sciences, Kwame Nkrumah University of Science and Technology, Kumasi, Ghana
,
Samuel Oppong Bekoe
3   Department of Pharmaceutical Chemistry, Faculty of Pharmacy and Pharmaceutical Sciences, Kwame Nkrumah University of Science and Technology, Kumasi, Ghana
,
Samuel Asare-Nkansah
3   Department of Pharmaceutical Chemistry, Faculty of Pharmacy and Pharmaceutical Sciences, Kwame Nkrumah University of Science and Technology, Kumasi, Ghana
,
Ina Kralisch
4   Chemical and Veterinary Inspection Office, Münsterland-Emscher-Lippe (CVUA-MEL) – AöR, Münster, Germany
,
Jonathan Jato
1   Institute of Pharmaceutical Biology and Phytochemistry, University of Münster, Münster, Germany
5   Department of Pharmacognosy and Herbal Medicine, School of Pharmacy, University of Health and Allied Sciences, Ho, Ghana
,
Verena Spiegler
1   Institute of Pharmaceutical Biology and Phytochemistry, University of Münster, Münster, Germany
,
Christian Agyare
6   Department of Pharmaceutics, Faculty of Pharmacy and Pharmaceutical Sciences, Kwame Nkrumah University of Science and Technology, Kumasi, Ghana
,
Emelia Oppong Bekoe
7   Department of Pharmacognosy and Herbal Medicine, School of Pharmacy, University of Ghana, Legon, Ghana
,
Andreas Hensel 
1   Institute of Pharmaceutical Biology and Phytochemistry, University of Münster, Münster, Germany
› Author AffiliationsSupported by: Deutsche Forschungsgemeinschaft Project 423277515 (HE1642/12-1) to EOB and AH
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Abstract

Herbal medicines are invaluable in African medicine, but quality and safety are not documented in many cases. Besides controlled farming, validated quality control methods are needed to ensure identity, purity, and content. Analytical specifications within modern monographs are needed for consistent batch quality. Combretum mucronatum leaves are widely used in West Africa, but state-of-the-art quality control methods and specifications are non-existent. The aim of the following study was the development of ICH-validated chromatographic protocols for identity, purity, content assay, and analytical specifications for consideration into pharmacopoeial monographs. UPLC-ESI-Q-TOF-MS/MS was used for untargeted phytochemical information on composition. Optimisation of extraction was based on phytochemical profiling. HPTLC was used for differentiation of C. mucronatum from other Combretum species and UPLC for simultaneous determination of 7 marker compounds. C. mucronatum batch analyses (n = 49) investigated the influence of harvest time and geographical origin. Pesticides screening from a 349-compound panel were carried out. 30 compounds, identified by LC-MS, were used for characterization of the plant material. Orietin, isoorientin, vitexin and isovitexin were used as specific marker compounds for qualitative and quantitative HPTLC purposes, while UPLC quantified additionally epicatechin, procyanidins B2 and C1. Influence of harvest time and geographic origin on the content of marker compounds was observed. Differences in the metabolite profiles of C. mucronatum compared to related Combretum species were established for quality control purposes. Contamination with high amoounts of chlorpyrifos, and folpet (sum of folpet and phtalimide, expressed as folpet) were also observed.

The study provides analytical protocols, analytical specifications and a drafted monograph for consideration for African pharmacopoeias, and reveals potential challenges in the quality of C. mucronatum.

Key words

Combretum mucronatum - Combretaceae - phytochemistry - quality control - specifications - analytical method validation - contaminants - metabolomics - design of experiment

Supporting Information

    The morphology of Combretum mucronatum is displayed within the Supporting Information #1; additionally the sutructural features of the typical marker compounds, 3D response plots for the optimization studies, the geographical locations of the collecting places, the Box-Behnken surface outcomes, the reference standards with analytical data for assessment of pesticides residues can be found in Supporting Information #1.

  • Supporting Information #1

    A draft of a monograph for Combretum mucronatum, including quality specifications and methodology for potential inclusion into a pharmacopoeia is presented in the Supporting Information #2.

  • Supporting Information #2


Publication History

Received: 21 September 2022

Accepted after revision: 20 December 2022

Accepted Manuscript online:
20 December 2022

Article published online:
10 March 2023

© 2023. Thieme. All rights reserved.

Georg Thieme Verlag KG
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