Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS
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 analy...
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| Format: | Article |
| Language: | English |
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MDPI AG
2022-09-01
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| Series: | Toxins |
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| Online Access: | https://www.mdpi.com/2072-6651/14/10/650 |
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| author | Lorena González-Gómez Sonia Morante-Zarcero Jorge A. M. Pereira José S. Câmara Isabel Sierra |
| author_facet | Lorena González-Gómez Sonia Morante-Zarcero Jorge A. M. Pereira José S. Câmara Isabel Sierra |
| author_sort | Lorena González-Gómez |
| collection | DOAJ |
| description | 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 (<i>Brugmansia versicolor</i>, <i>Solandra maxima,</i> and <i>Convolvulus arvensis</i>). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of <i>B. versicolor</i>. The highest concentration of atropine was found in flowers of <i>S. maxima</i> (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with <i>B. versicolor</i> and <i>S. maxima</i> 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. |
| first_indexed | 2024-03-09T19:25:36Z |
| format | Article |
| id | doaj.art-28bdb17bfa074f72bdf035b57b05dc2f |
| institution | Directory Open Access Journal |
| issn | 2072-6651 |
| language | English |
| last_indexed | 2024-03-09T19:25:36Z |
| publishDate | 2022-09-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Toxins |
| spelling | doaj.art-28bdb17bfa074f72bdf035b57b05dc2f2023-11-24T02:58:24ZengMDPI AGToxins2072-66512022-09-01141065010.3390/toxins14100650Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MSLorena González-Gómez0Sonia Morante-Zarcero1Jorge A. M. Pereira2José S. Câmara3Isabel Sierra4ESCET—Escuela Superior de Ciencias Experimentales y Tecnología, Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, C/Tulipán s/n, 28933 Móstoles, Madrid, SpainESCET—Escuela Superior de Ciencias Experimentales y Tecnología, Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, C/Tulipán s/n, 28933 Móstoles, Madrid, SpainCQM—Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105 Funchal, PortugalCQM—Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105 Funchal, PortugalESCET—Escuela Superior de Ciencias Experimentales y Tecnología, Departamento de Tecnología Química y Ambiental, Universidad Rey Juan Carlos, C/Tulipán s/n, 28933 Móstoles, Madrid, SpainThis 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 (<i>Brugmansia versicolor</i>, <i>Solandra maxima,</i> and <i>Convolvulus arvensis</i>). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of <i>B. versicolor</i>. The highest concentration of atropine was found in flowers of <i>S. maxima</i> (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with <i>B. versicolor</i> and <i>S. maxima</i> 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.https://www.mdpi.com/2072-6651/14/10/650atropinescopolaminetropane alkaloidsµ-QuEChERSHPLC-MS/MSleafy vegetables |
| spellingShingle | Lorena González-Gómez Sonia Morante-Zarcero Jorge A. M. Pereira José S. Câmara Isabel Sierra Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS Toxins atropine scopolamine tropane alkaloids µ-QuEChERS HPLC-MS/MS leafy vegetables |
| title | Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS |
| title_full | Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS |
| title_fullStr | Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS |
| title_full_unstemmed | Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS |
| title_short | Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS |
| title_sort | improved analytical approach for determination of tropane alkaloids in leafy vegetables based on µ quechers combined with hplc ms ms |
| topic | atropine scopolamine tropane alkaloids µ-QuEChERS HPLC-MS/MS leafy vegetables |
| url | https://www.mdpi.com/2072-6651/14/10/650 |
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