Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity
The research into new pharmaceutical substances based on essential oils, individual biologically active phytochemicals, and plant extracts is a priority in field of pharmaceutical sciences. A novel multicomponent substance based on <i>Melaleuca alternifolia</i> (<i>M. alternifolia&...
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-10-01
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| Series: | Antibiotics |
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| Online Access: | https://www.mdpi.com/2079-6382/12/10/1558 |
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| author | Viktor A. Filatov Egor A. Ilin Olesya Yu. Kulyak Elena I. Kalenikova |
| author_facet | Viktor A. Filatov Egor A. Ilin Olesya Yu. Kulyak Elena I. Kalenikova |
| author_sort | Viktor A. Filatov |
| collection | DOAJ |
| description | The research into new pharmaceutical substances based on essential oils, individual biologically active phytochemicals, and plant extracts is a priority in field of pharmaceutical sciences. A novel multicomponent substance based on <i>Melaleuca alternifolia</i> (<i>M. alternifolia</i>) leaf oil (TTO), 1,8-cineole (eucalyptol), and (-)-α-bisabolol with potent synergetic antimicrobial activity was investigated and suggested for the treatment of seborrheic dermatitis (SD) and dandruff. The objective of this research was to establish and validate a specific, accurate, and precise gas chromatography–mass spectrometry (GC–MS) method for further quantitative and qualitative analysis in order to ensure quality control. The main parameters of validation were suitability, specificity, linearity, accuracy, and intermediate precision according to the <i>European Pharmacopoeia</i> (XI edition), <i>Russian Pharmacopoeia</i> (XIV edition), and some parameters of ICH requirements. The peaks of fifteen chemical phytoconstituents were identified in the test sample solution with the prevalence of (−)-α-bisabolol (27.67%), 1,8-cineole (25.63%), and terpinen-4-ol (16.98%). These phytochemicals in the novel substance were chosen for standardization and validation of the GC–MS method. The chosen chromatographic conditions were confirmed for testing of the plant-based substance in a suitability test. It was established that the GC–MS method provides a significant separation, symmetry of peaks and resolution between phytochemicals. The calibration curves of each phytochemical had good linearity (R<sup>2</sup> > 0.999) in five concentrations. In the same concertation range, the accuracy of terpinen-4-ol, 1,8-cineol, and (−)-α-bisabolol determination using the method of additives was 98.3–101.60%; the relative standard deviation (RSD) ranged from 0.89% to 1.51% and corresponded to requirements. The intraday and interday precision was ≤2.56%. Thus, the GC–MS method was validated to be specific, sensitive, linear, accurate, and precise. This GC–MS method could be recommended as a routine analytic technique for multicomponent plant-based substances-enriched terpenes. |
| first_indexed | 2024-03-10T21:29:51Z |
| format | Article |
| id | doaj.art-e37920b831a940dfb11904c78290ddea |
| institution | Directory Open Access Journal |
| issn | 2079-6382 |
| language | English |
| last_indexed | 2024-03-10T21:29:51Z |
| publishDate | 2023-10-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Antibiotics |
| spelling | doaj.art-e37920b831a940dfb11904c78290ddea2023-11-19T15:27:10ZengMDPI AGAntibiotics2079-63822023-10-011210155810.3390/antibiotics12101558Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial ActivityViktor A. Filatov0Egor A. Ilin1Olesya Yu. Kulyak2Elena I. Kalenikova3Department of Pharmaceutical Chemistry and Organization of Pharmaceutical Business, Faculty of Basic Medicine, Lomonosov Moscow State University, 119991 Moscow, RussiaDepartment of Chemistry, Lomonosov Moscow State University, 119991 Moscow, RussiaDepartment of Pharmaceutical Chemistry and Organization of Pharmaceutical Business, Faculty of Basic Medicine, Lomonosov Moscow State University, 119991 Moscow, RussiaDepartment of Pharmaceutical Chemistry and Organization of Pharmaceutical Business, Faculty of Basic Medicine, Lomonosov Moscow State University, 119991 Moscow, RussiaThe research into new pharmaceutical substances based on essential oils, individual biologically active phytochemicals, and plant extracts is a priority in field of pharmaceutical sciences. A novel multicomponent substance based on <i>Melaleuca alternifolia</i> (<i>M. alternifolia</i>) leaf oil (TTO), 1,8-cineole (eucalyptol), and (-)-α-bisabolol with potent synergetic antimicrobial activity was investigated and suggested for the treatment of seborrheic dermatitis (SD) and dandruff. The objective of this research was to establish and validate a specific, accurate, and precise gas chromatography–mass spectrometry (GC–MS) method for further quantitative and qualitative analysis in order to ensure quality control. The main parameters of validation were suitability, specificity, linearity, accuracy, and intermediate precision according to the <i>European Pharmacopoeia</i> (XI edition), <i>Russian Pharmacopoeia</i> (XIV edition), and some parameters of ICH requirements. The peaks of fifteen chemical phytoconstituents were identified in the test sample solution with the prevalence of (−)-α-bisabolol (27.67%), 1,8-cineole (25.63%), and terpinen-4-ol (16.98%). These phytochemicals in the novel substance were chosen for standardization and validation of the GC–MS method. The chosen chromatographic conditions were confirmed for testing of the plant-based substance in a suitability test. It was established that the GC–MS method provides a significant separation, symmetry of peaks and resolution between phytochemicals. The calibration curves of each phytochemical had good linearity (R<sup>2</sup> > 0.999) in five concentrations. In the same concertation range, the accuracy of terpinen-4-ol, 1,8-cineol, and (−)-α-bisabolol determination using the method of additives was 98.3–101.60%; the relative standard deviation (RSD) ranged from 0.89% to 1.51% and corresponded to requirements. The intraday and interday precision was ≤2.56%. Thus, the GC–MS method was validated to be specific, sensitive, linear, accurate, and precise. This GC–MS method could be recommended as a routine analytic technique for multicomponent plant-based substances-enriched terpenes.https://www.mdpi.com/2079-6382/12/10/1558tea tree essential oileucalyptolbisabololterpenesGC–MSvalidation |
| spellingShingle | Viktor A. Filatov Egor A. Ilin Olesya Yu. Kulyak Elena I. Kalenikova Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity Antibiotics tea tree essential oil eucalyptol bisabolol terpenes GC–MS validation |
| title | Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity |
| title_full | Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity |
| title_fullStr | Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity |
| title_full_unstemmed | Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity |
| title_short | Development and Validation of a Gas Chromatography–Mass Spectrometry Method for the Analysis of the Novel Plant-Based Substance with Antimicrobial Activity |
| title_sort | development and validation of a gas chromatography mass spectrometry method for the analysis of the novel plant based substance with antimicrobial activity |
| topic | tea tree essential oil eucalyptol bisabolol terpenes GC–MS validation |
| url | https://www.mdpi.com/2079-6382/12/10/1558 |
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