Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements
Two LC methods were developed for the achiral and chiral reversed-phase (RP) analysis of an amino acid (AA) pool in a food supplement, in compliance with the main paradigms of Green Chromatography. A direct achiral ion-pairing RP-HPLC method was optimized under gradient conditions with a water-ethan...
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MDPI AG
2022-11-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/27/22/7724 |
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| author | Ina Varfaj Andrea Carotti Luciano Mangiapelo Lina Cossignani Agnese Taticchi Antonio Macchiarulo Federica Ianni Roccaldo Sardella |
| author_facet | Ina Varfaj Andrea Carotti Luciano Mangiapelo Lina Cossignani Agnese Taticchi Antonio Macchiarulo Federica Ianni Roccaldo Sardella |
| author_sort | Ina Varfaj |
| collection | DOAJ |
| description | Two LC methods were developed for the achiral and chiral reversed-phase (RP) analysis of an amino acid (AA) pool in a food supplement, in compliance with the main paradigms of Green Chromatography. A direct achiral ion-pairing RP-HPLC method was optimized under gradient conditions with a water-ethanol (EtOH) eluent containing heptafluorobutyric acid (0.1%, <i>v/v</i>), to quantify the eight essential AAs (Ile, Leu, Lys, Met, Phe, Thr, Trp, and Val) contained in the food supplement. Thus, the usually employed acetonitrile was profitably substituted with the less toxic and more benign EtOH. The method was validated for Leu and Phe. The chiral LC method performed with a teicoplanin chiral stationary phase was developed with a water-EtOH (60:40, <i>v/v</i>) eluent with 0.1%, <i>v/v</i> acetic acid. The enantioselective analysis was carried out without any prior derivatization step. Both developed methods performed highly for all eight AAs and revealed that: (i) the content of six out of eight AAs was consistent with the manufacturer declaration; (ii) only L-AAs were present. Furthermore, it was demonstrated that a two-dimensional achiral–chiral configuration is possible in practice, making it even more environmentally sustainable. A molecular modelling investigation revealed interesting insights into the enantiorecognition mechanism of Lys. |
| first_indexed | 2024-03-09T18:07:40Z |
| format | Article |
| id | doaj.art-226953d842f34e7ebdd9577e55f84b78 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-09T18:07:40Z |
| publishDate | 2022-11-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-226953d842f34e7ebdd9577e55f84b782023-11-24T09:20:04ZengMDPI AGMolecules1420-30492022-11-012722772410.3390/molecules27227724Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food SupplementsIna Varfaj0Andrea Carotti1Luciano Mangiapelo2Lina Cossignani3Agnese Taticchi4Antonio Macchiarulo5Federica Ianni6Roccaldo Sardella7Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Agricultural Food and Environmental Sciences, University of Perugia, Via S. Costanzo, 06126 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyDepartment of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia, ItalyTwo LC methods were developed for the achiral and chiral reversed-phase (RP) analysis of an amino acid (AA) pool in a food supplement, in compliance with the main paradigms of Green Chromatography. A direct achiral ion-pairing RP-HPLC method was optimized under gradient conditions with a water-ethanol (EtOH) eluent containing heptafluorobutyric acid (0.1%, <i>v/v</i>), to quantify the eight essential AAs (Ile, Leu, Lys, Met, Phe, Thr, Trp, and Val) contained in the food supplement. Thus, the usually employed acetonitrile was profitably substituted with the less toxic and more benign EtOH. The method was validated for Leu and Phe. The chiral LC method performed with a teicoplanin chiral stationary phase was developed with a water-EtOH (60:40, <i>v/v</i>) eluent with 0.1%, <i>v/v</i> acetic acid. The enantioselective analysis was carried out without any prior derivatization step. Both developed methods performed highly for all eight AAs and revealed that: (i) the content of six out of eight AAs was consistent with the manufacturer declaration; (ii) only L-AAs were present. Furthermore, it was demonstrated that a two-dimensional achiral–chiral configuration is possible in practice, making it even more environmentally sustainable. A molecular modelling investigation revealed interesting insights into the enantiorecognition mechanism of Lys.https://www.mdpi.com/1420-3049/27/22/7724enantiorecognition mechanismgreen chromatographyion-pairing agentteicoplanin-based stationary phase |
| spellingShingle | Ina Varfaj Andrea Carotti Luciano Mangiapelo Lina Cossignani Agnese Taticchi Antonio Macchiarulo Federica Ianni Roccaldo Sardella Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements Molecules enantiorecognition mechanism green chromatography ion-pairing agent teicoplanin-based stationary phase |
| title | Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements |
| title_full | Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements |
| title_fullStr | Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements |
| title_full_unstemmed | Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements |
| title_short | Environmentally Sustainable Achiral and Chiral Chromatographic Analysis of Amino Acids in Food Supplements |
| title_sort | environmentally sustainable achiral and chiral chromatographic analysis of amino acids in food supplements |
| topic | enantiorecognition mechanism green chromatography ion-pairing agent teicoplanin-based stationary phase |
| url | https://www.mdpi.com/1420-3049/27/22/7724 |
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