Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins
Lupin alkaloids (LAs) represent a class of toxic secondary metabolites in plants, in particular in <i>Lupinus</i> spp.; they are produced as a defense mechanism due to their strong bitter taste and are very dangerous for human and animals. In this work, a sensitive and reliable high perf...
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MDPI AG
2023-02-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/28/4/1531 |
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| author | Fabiola Eugelio Sara Palmieri Federico Fanti Luana Messuri Alessia Pepe Dario Compagnone Manuel Sergi |
| author_facet | Fabiola Eugelio Sara Palmieri Federico Fanti Luana Messuri Alessia Pepe Dario Compagnone Manuel Sergi |
| author_sort | Fabiola Eugelio |
| collection | DOAJ |
| description | Lupin alkaloids (LAs) represent a class of toxic secondary metabolites in plants, in particular in <i>Lupinus</i> spp.; they are produced as a defense mechanism due to their strong bitter taste and are very dangerous for human and animals. In this work, a sensitive and reliable high performance liquid chromatography—tandem mass spectrometry (HPLC-MS/MS) analytical method for the identification and quantification of thirteen lupin alkaloids was developed and validated according to FDA guidelines. Efficient extraction and clean-up steps, carried out by solid-phase extraction, were finely tuned on the basis of the characteristics of the analytes and lupin samples, providing good selectivity with minimized matrix interference. The effectiveness of the method was proven by the satisfactory recovery values obtained for most of the analytes and a matrix effect ≤23% for all tested levels. In addition, a sensitive and reliable determination of the target compounds was obtained; LOQs were between 1 and 25 µg Kg<sup>−1</sup>, i.e., below the requested maximum levels (<200 mg Kg<sup>−1</sup>). The method was applied to evaluate the LAs profile in different batches of raw <i>L. albus</i> L. samples, varying in size and across farming treatments. |
| first_indexed | 2024-03-11T08:21:52Z |
| format | Article |
| id | doaj.art-259147136f2d472497e6af65a0e04e22 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-11T08:21:52Z |
| publishDate | 2023-02-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-259147136f2d472497e6af65a0e04e222023-11-16T22:19:46ZengMDPI AGMolecules1420-30492023-02-01284153110.3390/molecules28041531Development of an HPLC-MS/MS Method for the Determination of Alkaloids in LupinsFabiola Eugelio0Sara Palmieri1Federico Fanti2Luana Messuri3Alessia Pepe4Dario Compagnone5Manuel Sergi6Department of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Bioscience and Technology for Food, Agriculture and Environment, University of Teramo, Via Renato Balzarini 1, 64100 Teramo, ItalyDepartment of Chemistry, Sapienza University of Rome, Piazzale Aldo Moro 5, 00185 Rome, ItalyLupin alkaloids (LAs) represent a class of toxic secondary metabolites in plants, in particular in <i>Lupinus</i> spp.; they are produced as a defense mechanism due to their strong bitter taste and are very dangerous for human and animals. In this work, a sensitive and reliable high performance liquid chromatography—tandem mass spectrometry (HPLC-MS/MS) analytical method for the identification and quantification of thirteen lupin alkaloids was developed and validated according to FDA guidelines. Efficient extraction and clean-up steps, carried out by solid-phase extraction, were finely tuned on the basis of the characteristics of the analytes and lupin samples, providing good selectivity with minimized matrix interference. The effectiveness of the method was proven by the satisfactory recovery values obtained for most of the analytes and a matrix effect ≤23% for all tested levels. In addition, a sensitive and reliable determination of the target compounds was obtained; LOQs were between 1 and 25 µg Kg<sup>−1</sup>, i.e., below the requested maximum levels (<200 mg Kg<sup>−1</sup>). The method was applied to evaluate the LAs profile in different batches of raw <i>L. albus</i> L. samples, varying in size and across farming treatments.https://www.mdpi.com/1420-3049/28/4/1531alkaloidsHPLC-MS/MSsolid-phase extractionlupins<i>Lupinus albus</i> L. |
| spellingShingle | Fabiola Eugelio Sara Palmieri Federico Fanti Luana Messuri Alessia Pepe Dario Compagnone Manuel Sergi Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins Molecules alkaloids HPLC-MS/MS solid-phase extraction lupins <i>Lupinus albus</i> L. |
| title | Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins |
| title_full | Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins |
| title_fullStr | Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins |
| title_full_unstemmed | Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins |
| title_short | Development of an HPLC-MS/MS Method for the Determination of Alkaloids in Lupins |
| title_sort | development of an hplc ms ms method for the determination of alkaloids in lupins |
| topic | alkaloids HPLC-MS/MS solid-phase extraction lupins <i>Lupinus albus</i> L. |
| url | https://www.mdpi.com/1420-3049/28/4/1531 |
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