Development and validation of an analytical method based on QuEChERS followed by UHPLC–ToF-MS for the determination of tropane alkaloids in buckwheat (Fagopyrum esculentum L.) and buckwheat products

Abstract

A method was developed for the determination of tropane alkaloids (TAs), including atropine, scopolamine, anisodamine and homatropine in buckwheat and related products. This work presents an optimised methodology based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure followed by ultra-high performance liquid chromatography combined with time-of-flight mass spectrometry for the determination of TAs (atropine, scopolamine, anisodamine and homatropine) in buckwheat samples. The analytical methodology was successfully validated, demonstrating good linearity, low limit of quantification, repeatability (RSD_r < 15%), inter-day precision (RSD_R < 19%) and recovery (74–113%). Finally, 13 commercial samples of buckwheat were analysed and the results demonstrated that they were in compliance with the current European regulations regarding TAs.

Keywords:

• Plant toxins
• buckwheat
• food safety
• analytical validation

Author contributions

ARSM: Methodology, software, validation, formal analysis, investigation, data curation, visualisation, writing—original draft. CC: Methodology, validation, investigation. SB: Writing—review and editing; AP: Supervision, writing—review and editing. ASS: Conceptualisation, methodology, investigation, resources, data curation, writing—review and editing, supervision, funding acquisition. All authors have read and agreed to the published version of the manuscript.

Disclosure statement

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

Additional information

Funding

This work was financially supported by the research project ValICET (PRIMA/0001/2020)—Valorise foods and Improve Competitiveness through Emerging Technologies applied to food by products within the circular economy framework (section 2 PRIMA project) funded in Portugal by Foundation for Science and Technology (FCT) (doi:10.54499/PRIMA/0001/2020). The work was supported by UIDB/00211/2020 with funding from FCT/MCTES through national funds. ARSM would like to thank to FCT for her fellowship (2023.04705.BDANA).