An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices
Patulin (PAT) is a mycotoxin produced in fruits, especially in apples, by diverse fungal species that can be transferred into industrial apple juice during processing. An accurate, effective, and selective method has been validated for the quantification of PAT in different commercial apple juices b...
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| Format: | Article |
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MDPI AG
2023-02-01
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| Series: | Separations |
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| Online Access: | https://www.mdpi.com/2297-8739/10/3/149 |
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| author | José S. Câmara Paulo Fernandes Nelson Barros Rosa Perestrelo |
| author_facet | José S. Câmara Paulo Fernandes Nelson Barros Rosa Perestrelo |
| author_sort | José S. Câmara |
| collection | DOAJ |
| description | Patulin (PAT) is a mycotoxin produced in fruits, especially in apples, by diverse fungal species that can be transferred into industrial apple juice during processing. An accurate, effective, and selective method has been validated for the quantification of PAT in different commercial apple juices by combining a modified µ-QuEChERS procedure with high-pressure liquid chromatography (LC) equipped with a triple quadrupole mass spectrometer (QqQMS). This sample extraction procedure reduced interference from the sugar-rich matrix, and the separation was performed using the C18 Atlantis T3 column within 10 min. PAT was found by MS with electrospray negative ionization (ESI<sup>−</sup>) in the mode of multiple reaction monitoring (MRM). The correlation coefficient (R<sup>2</sup> = 0.999) satisfied the prerequisite of linearity for PAT in the concentration range of 2–50 μg/kg. The limits of detection (LOD) and quantification (LOQ) of PAT were 0.32 and 1.15 μg/kg, respectively, which were compliant with the maximum levels settled in Commission Regulation (EC) No. 1881/2006. The recoveries were within the 92–103% range, at three fortified levels of 2, 20 and 50 μg/kg, with relative standard deviations lower than 7%. Based on analytical validation, it was confirmed that the µ-QuEChERS/HPLC-MS/MS method is an enhanced, reliable, and quick approach for determination of PAT in apple juice. The current approach proposes reduced sample preparation and analysis time. In addition, it is economical, environmentally friendly, and simpler to implement in comparison to traditional approaches. |
| first_indexed | 2024-03-11T05:55:17Z |
| format | Article |
| id | doaj.art-64fac8cb06a14e0b85a2a392b59a630a |
| institution | Directory Open Access Journal |
| issn | 2297-8739 |
| language | English |
| last_indexed | 2024-03-11T05:55:17Z |
| publishDate | 2023-02-01 |
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| record_format | Article |
| series | Separations |
| spelling | doaj.art-64fac8cb06a14e0b85a2a392b59a630a2023-11-17T13:49:44ZengMDPI AGSeparations2297-87392023-02-0110314910.3390/separations10030149An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple JuicesJosé S. Câmara0Paulo Fernandes1Nelson Barros2Rosa Perestrelo3CQM—Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105 Funchal, PortugalLaboratório Regional de Veterinária e Segurança Alimentar, Caminho das Quebradas de Baixo, 9000-254 Funchal, PortugalLaboratório Regional de Veterinária e Segurança Alimentar, Caminho das Quebradas de Baixo, 9000-254 Funchal, PortugalCQM—Centro de Química da Madeira, Universidade da Madeira, Campus da Penteada, 9020-105 Funchal, PortugalPatulin (PAT) is a mycotoxin produced in fruits, especially in apples, by diverse fungal species that can be transferred into industrial apple juice during processing. An accurate, effective, and selective method has been validated for the quantification of PAT in different commercial apple juices by combining a modified µ-QuEChERS procedure with high-pressure liquid chromatography (LC) equipped with a triple quadrupole mass spectrometer (QqQMS). This sample extraction procedure reduced interference from the sugar-rich matrix, and the separation was performed using the C18 Atlantis T3 column within 10 min. PAT was found by MS with electrospray negative ionization (ESI<sup>−</sup>) in the mode of multiple reaction monitoring (MRM). The correlation coefficient (R<sup>2</sup> = 0.999) satisfied the prerequisite of linearity for PAT in the concentration range of 2–50 μg/kg. The limits of detection (LOD) and quantification (LOQ) of PAT were 0.32 and 1.15 μg/kg, respectively, which were compliant with the maximum levels settled in Commission Regulation (EC) No. 1881/2006. The recoveries were within the 92–103% range, at three fortified levels of 2, 20 and 50 μg/kg, with relative standard deviations lower than 7%. Based on analytical validation, it was confirmed that the µ-QuEChERS/HPLC-MS/MS method is an enhanced, reliable, and quick approach for determination of PAT in apple juice. The current approach proposes reduced sample preparation and analysis time. In addition, it is economical, environmentally friendly, and simpler to implement in comparison to traditional approaches.https://www.mdpi.com/2297-8739/10/3/149mycotoxinpatulinapple juiceµ-QuEChERSLC-MS/MS |
| spellingShingle | José S. Câmara Paulo Fernandes Nelson Barros Rosa Perestrelo An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices Separations mycotoxin patulin apple juice µ-QuEChERS LC-MS/MS |
| title | An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices |
| title_full | An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices |
| title_fullStr | An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices |
| title_full_unstemmed | An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices |
| title_short | An Improved Analytical Approach Based on µ-QuEChERS Combined with LC-ESI/MS for Monitoring the Occurrence and Levels of Patulin in Commercial Apple Juices |
| title_sort | improved analytical approach based on µ quechers combined with lc esi ms for monitoring the occurrence and levels of patulin in commercial apple juices |
| topic | mycotoxin patulin apple juice µ-QuEChERS LC-MS/MS |
| url | https://www.mdpi.com/2297-8739/10/3/149 |
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