Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS

Lorena González-Gómez; Sonia Morante-Zarcero; Jorge A M Pereira; José S Câmara; Isabel Sierra

doi:10.3390/toxins14100650

Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS

Toxins (Basel). 2022 Sep 20;14(10):650. doi: 10.3390/toxins14100650.

Authors

Lorena González-Gómez^{1

2}, Sonia Morante-Zarcero¹, Jorge A M Pereira², José S Câmara^{2

3}, Isabel Sierra¹

Affiliations

¹ ESCET-Escuela Superior de Ciencias Experimentales y Tecnología, Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, C/Tulipán s/n, 28933 Móstoles, Madrid, Spain.
² CQM-Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105 Funchal, Portugal.
³ Departamento de Química, Faculdade de Ciências Exatas e da Engenharia, Universidade da Madeira, Campus Universitário da Penteada, 9020-105 Funchal, Portugal.

Abstract

This work presents an optimized methodology based on the miniaturization of the original QuEChERS (μ-QuEChERS) followed by liquid chromatography coupled to mass spectrometry (HPLC-MS/MS) for the determination of tropane alkaloids (TAs), atropine, and scopolamine in leafy vegetable samples. The analytical methodology was successfully validated, demonstrating quantitation limits (MQL) ≤ 2.3 ng/g, good accuracy, and precision, with recoveries between 90-100% and RSD ≤ 13% for both analytes. The method was applied to the analysis of TA-producing plants (Brugmansia versicolor, Solandra maxima, and Convolvulus arvensis). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of B. versicolor. The highest concentration of atropine was found in flowers of S. maxima (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with B. versicolor and S. maxima were analysed to verify the efficacy of the method, showing recoveries between 82 and 110% for both analytes. Finally, the method was applied to the analysis of eighteen samples of leafy vegetables, finding atropine in three samples of mixed leafy vegetables, with concentrations of 2.7, 3.2, and 3.4 ng/g, and in nine samples with concentrations ≤MQL. In turn, scopolamine was only found in a sample of chopped Swiss chard with a concentration ≤MQL.

Keywords: HPLC-MS/MS; atropine; leafy vegetables; scopolamine; tropane alkaloids; µ-QuEChERS.

Publication types

Research Support, Non-U.S. Gov't

MeSH terms

Atropine
Chromatography, High Pressure Liquid
Plant Leaves / chemistry
Scopolamine / analysis
Tandem Mass Spectrometry* / methods
Tropanes / analysis
Vegetables* / chemistry

Substances

Tropanes
Atropine
Scopolamine

Grants and funding

This research was funded by MCIU/AEI/FEDER, UE, project number RTI2018-094558-B-I00 (EVALKALIM). This work was also funded by FCT-Fundação para a Ciência e a Tecnologia through the CQM Base Fund—UIDB/00674/2020, and Programmatic Fund—UIDP/00674/2020, and by ARDITI-Agência Regional para o Desenvolvimento da Investigação Tecnologia e Inovação, through the project M1420-01-0145-FEDER-000005—Centro de Química da Madeira—CQM+ (Madeira 14-20 Program) and the Project M1420–09–5369-FSE-000001 for the Post-Doctoral fellowship given to J.A.M.P. The authors also acknowledge the financial support from Fundação para a Ciência e Tecnologia and Madeira 14-2020 program to the Portuguese Mass Spectrometry Network through PROEQUIPRAM program, M14-20 M1420-01-0145-FEDER-000008.