Validating a sensitive LCMS method for the quantitation of artemisinin in Artemisia spp. including material used in retracted clinical trials

• Published in: Journal of pharmaceutical and biomedical analysis Vol. 208; p. 114446
• Main Authors: Lee, Barend J., van Niekerk, Suzanne E., Legoabe, Lesetja J., van der Kooy, Frank
• Format: Journal Article
• Language: English
• Published: England Elsevier B.V 20-01-2022
• Subjects: Artemisia; Artemisia afra; Artemisia annua; Artemisinin; Artemisinins - analysis; Chromatography, Liquid; Clinical Trials as Topic; Humans; LCMS; Mass Spectrometry; Plant Extracts; Quality control; Young Adult; Artemisia afra; Artemisia annua; LCMS; Artemisinin; Quality control
• DOI: 10.1016/j.jpba.2021.114446
• EISSN: 1873-264X
• ISSN: 0731-7085

•A sensitive LCMS method was developed for the quantitation of artemisinin in Artemisia annua and A. afra.•This method was applied to a collection of Artemisia samples including two A. afra samples used in retracted clinical trials.•No artemisinin could be detected in any A. afra samples except in the samples used in the clinical trials.•Quality control of herbal material is of utmost importance to ensure the safety of trial participants.
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Two recent clinical trials reported that Artemisia afra contained significant amounts of the bioactive compound artemisinin. We suspected sample contamination and therefore obtained the A. afra material for testing. A sensitive liquid chromatography mass spectrometry method was developed and validated for the accurate quantitation of artemisinin in Artemisia annua and A. afra plant material. This validated analytical method, with a limit of detection of 0.22 ng/mL (0.22 pg on column), which is an order of magnitude more sensitive than recently published methods, was applied to quantify artemisinin in a collection of Artemisia samples including the A. afra material that was used in the clinical trials.All 16A. annua samples (oldest sample 21 years old) contained the expected levels of artemisinin (0.12–0.63%) whilst none of the A. afra samples in our collection contained any trace of artemisinin (> 0.00001%). However, the A. afra samples used in the clinical trials did contain detectable amounts of artemisinin (0.0013% and 0.0011% vs the claimed amount of 0.0045%).The authors of the clinical trials suspected that cross contamination during sample handling and preparation was likely, reconfirming the importance of having analytical quality control methods in place before clinical trials are conducted. Quality control and ensuring safety of trial participants is of utmost importance.