Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds
A solid-phase extraction (SPE) technique was developed and optimised for isolation and concentration of extractable and bound phenolic acids from germinated spelt seeds, for analysis by liquid chromatography–mass spectrometry. Samples initially underwent solvent extraction under different conditions...
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| Format: | Article |
| Language: | English |
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MDPI AG
2021-07-01
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| Series: | Antioxidants |
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| Online Access: | https://www.mdpi.com/2076-3921/10/7/1085 |
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| author | Marjeta Mencin Maja Mikulic-Petkovsek Robert Veberič Petra Terpinc |
| author_facet | Marjeta Mencin Maja Mikulic-Petkovsek Robert Veberič Petra Terpinc |
| author_sort | Marjeta Mencin |
| collection | DOAJ |
| description | A solid-phase extraction (SPE) technique was developed and optimised for isolation and concentration of extractable and bound phenolic acids from germinated spelt seeds, for analysis by liquid chromatography–mass spectrometry. Samples initially underwent solvent extraction under different conditions to maximise the yield of phenolic antioxidants. Optimal extraction conditions for extractable phenolics were absolute methanol as solvent, sample-to-methanol ratio 1:9, and reconstitution in non-acidified water. The bound phenolics were extracted from sample pellets using hydrolysis with 2 M NaOH, acidification of the hydrolysate with formic acid, and simultaneous isolation and purification using Strata X polymeric RP tubes. Compared to liquid-liquid extraction, this direct SPE protocol has significant advantages in terms of higher extraction efficiencies of total and individual phenolics and their antioxidant activities. These data suggest that direct SPE represents a rapid and reliable method for quantitative analysis of both the extractable and the commonly overlooked bound phenolics in <i>Triticum spelta</i> seeds. |
| first_indexed | 2024-03-10T09:47:21Z |
| format | Article |
| id | doaj.art-d2bd036c91b34fc19683126dda09fe48 |
| institution | Directory Open Access Journal |
| issn | 2076-3921 |
| language | English |
| last_indexed | 2024-03-10T09:47:21Z |
| publishDate | 2021-07-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Antioxidants |
| spelling | doaj.art-d2bd036c91b34fc19683126dda09fe482023-11-22T03:05:11ZengMDPI AGAntioxidants2076-39212021-07-01107108510.3390/antiox10071085Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) SeedsMarjeta Mencin0Maja Mikulic-Petkovsek1Robert Veberič2Petra Terpinc3Department of Food Science and Technology, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, SloveniaDepartment of Agronomy, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, SloveniaDepartment of Agronomy, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, SloveniaDepartment of Food Science and Technology, Biotechnical Faculty, University of Ljubljana, Jamnikarjeva 101, SI-1111 Ljubljana, SloveniaA solid-phase extraction (SPE) technique was developed and optimised for isolation and concentration of extractable and bound phenolic acids from germinated spelt seeds, for analysis by liquid chromatography–mass spectrometry. Samples initially underwent solvent extraction under different conditions to maximise the yield of phenolic antioxidants. Optimal extraction conditions for extractable phenolics were absolute methanol as solvent, sample-to-methanol ratio 1:9, and reconstitution in non-acidified water. The bound phenolics were extracted from sample pellets using hydrolysis with 2 M NaOH, acidification of the hydrolysate with formic acid, and simultaneous isolation and purification using Strata X polymeric RP tubes. Compared to liquid-liquid extraction, this direct SPE protocol has significant advantages in terms of higher extraction efficiencies of total and individual phenolics and their antioxidant activities. These data suggest that direct SPE represents a rapid and reliable method for quantitative analysis of both the extractable and the commonly overlooked bound phenolics in <i>Triticum spelta</i> seeds.https://www.mdpi.com/2076-3921/10/7/1085spelt phenolicsextractionhydrolysissolid-phase extractionliquid-liquid extractionantioxidant activity |
| spellingShingle | Marjeta Mencin Maja Mikulic-Petkovsek Robert Veberič Petra Terpinc Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds Antioxidants spelt phenolics extraction hydrolysis solid-phase extraction liquid-liquid extraction antioxidant activity |
| title | Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds |
| title_full | Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds |
| title_fullStr | Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds |
| title_full_unstemmed | Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds |
| title_short | Development and Optimisation of Solid-Phase Extraction of Extractable and Bound Phenolic Acids in Spelt (<i>Triticum spelta</i> L.) Seeds |
| title_sort | development and optimisation of solid phase extraction of extractable and bound phenolic acids in spelt i triticum spelta i l seeds |
| topic | spelt phenolics extraction hydrolysis solid-phase extraction liquid-liquid extraction antioxidant activity |
| url | https://www.mdpi.com/2076-3921/10/7/1085 |
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