Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples
Phomopsin A (PHO-A), a potent mycotoxin produced by the pathogenic fungus Diaporthe toxica, is a growing international concern due to the high toxicity and prevalence in lupin plants, a vital source of food and feed. This hexapeptide mycotoxin has raised health concerns for both animals and humans,...
| Main Authors: | , , , , , , , , |
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| Format: | Article |
| Language: | English |
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Elsevier
2024-05-01
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| Series: | Journal of Chromatography Open |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2772391723000336 |
| _version_ | 1797403588961501184 |
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| author | Fabiola Eugelio Sara Palmieri Federico Fanti Francesco Buccioni Eleonora Oliva Antonello Paparella Michele Del Carlo Dario Compagnone Manuel Sergi |
| author_facet | Fabiola Eugelio Sara Palmieri Federico Fanti Francesco Buccioni Eleonora Oliva Antonello Paparella Michele Del Carlo Dario Compagnone Manuel Sergi |
| author_sort | Fabiola Eugelio |
| collection | DOAJ |
| description | Phomopsin A (PHO-A), a potent mycotoxin produced by the pathogenic fungus Diaporthe toxica, is a growing international concern due to the high toxicity and prevalence in lupin plants, a vital source of food and feed. This hexapeptide mycotoxin has raised health concerns for both animals and humans, prompting regulatory bodies to set maximum allowable levels in lupin products.Different analytical methods have been developed for PHO-A detection, including Enzyme-Linked Immuno-Sorbent Assay (ELISA) and high-performance liquid chromatography (HPLC) coupled with different detectors; they often lack sensitivity and selectivity required to meet maximum regulatory limits (MRL). In this work, we present a robust and sensitive method for PHO-A quantification and determination, developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).This method incorporates a selective clean-up step using Micro Solid Phase Extraction (µ-SPE) to efficiently purify samples, ensuring a rapid, efficient, and selective recovery of PHO-A from the complex lupin matrix. The clean-up step not only helps in achieving lower detection limits but also minimizes matrix effects and contamination. The proposed method was validated following international guidelines, demonstrating reliable recovery, matrix effects, linearity, accuracy, and precision.Additionally, this method was successfully applied to artificially contaminated Lupinus albus L. samples, confirming the suitability for assessing PHO-A contamination. This analytical approach fills a critical gap in the literature by providing a specific, sensitive, and selective method for PHO-A analysis, contributing to the safety of lupin products and field monitoring. |
| first_indexed | 2024-03-09T02:41:36Z |
| format | Article |
| id | doaj.art-b5cfcdf8ed1c44d697bff3fd48fc2047 |
| institution | Directory Open Access Journal |
| issn | 2772-3917 |
| language | English |
| last_indexed | 2024-03-09T02:41:36Z |
| publishDate | 2024-05-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Journal of Chromatography Open |
| spelling | doaj.art-b5cfcdf8ed1c44d697bff3fd48fc20472023-12-06T04:17:55ZengElsevierJournal of Chromatography Open2772-39172024-05-015100109Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samplesFabiola Eugelio0Sara Palmieri1Federico Fanti2Francesco Buccioni3Eleonora Oliva4Antonello Paparella5Michele Del Carlo6Dario Compagnone7Manuel Sergi8Department 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, Italy; Corresponding author at: Department of Bioscience and Technologies for Food, Agriculture and Environment, University of Teramo, Via R. Balzarini, 1, 64100 Teramo TE, Italy.Department 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, ItalyPhomopsin A (PHO-A), a potent mycotoxin produced by the pathogenic fungus Diaporthe toxica, is a growing international concern due to the high toxicity and prevalence in lupin plants, a vital source of food and feed. This hexapeptide mycotoxin has raised health concerns for both animals and humans, prompting regulatory bodies to set maximum allowable levels in lupin products.Different analytical methods have been developed for PHO-A detection, including Enzyme-Linked Immuno-Sorbent Assay (ELISA) and high-performance liquid chromatography (HPLC) coupled with different detectors; they often lack sensitivity and selectivity required to meet maximum regulatory limits (MRL). In this work, we present a robust and sensitive method for PHO-A quantification and determination, developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).This method incorporates a selective clean-up step using Micro Solid Phase Extraction (µ-SPE) to efficiently purify samples, ensuring a rapid, efficient, and selective recovery of PHO-A from the complex lupin matrix. The clean-up step not only helps in achieving lower detection limits but also minimizes matrix effects and contamination. The proposed method was validated following international guidelines, demonstrating reliable recovery, matrix effects, linearity, accuracy, and precision.Additionally, this method was successfully applied to artificially contaminated Lupinus albus L. samples, confirming the suitability for assessing PHO-A contamination. This analytical approach fills a critical gap in the literature by providing a specific, sensitive, and selective method for PHO-A analysis, contributing to the safety of lupin products and field monitoring.http://www.sciencedirect.com/science/article/pii/S2772391723000336Phomopsin ALupinsMicro solid-phase extractionUHPLC-MS/MS |
| spellingShingle | Fabiola Eugelio Sara Palmieri Federico Fanti Francesco Buccioni Eleonora Oliva Antonello Paparella Michele Del Carlo Dario Compagnone Manuel Sergi Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples Journal of Chromatography Open Phomopsin A Lupins Micro solid-phase extraction UHPLC-MS/MS |
| title | Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples |
| title_full | Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples |
| title_fullStr | Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples |
| title_full_unstemmed | Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples |
| title_short | Development and validation of analytical method by micro-solid-phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of Phomopsin A in lupin samples |
| title_sort | development and validation of analytical method by micro solid phase extraction followed by ultra high performance liquid chromatography coupled to tandem mass spectrometry analysis for the quantification of phomopsin a in lupin samples |
| topic | Phomopsin A Lupins Micro solid-phase extraction UHPLC-MS/MS |
| url | http://www.sciencedirect.com/science/article/pii/S2772391723000336 |
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