The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS
Fatty acid analysis is an essential step in evaluating the potential of macroalgae for biodiesel production. An extraction method was developed to simultaneously analyze up to five types of biodiesel-fuel-related fatty acids (myristic acid, palmitic acid, <i>cis</i>-palmitvaccenic acid,...
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| Format: | Article |
| Language: | English |
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MDPI AG
2024-01-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/29/2/430 |
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| author | Taewoo Yum Eun-Yong Kim Yeongeun Kim Sukyoung Choi Ki-Jung Paeng |
| author_facet | Taewoo Yum Eun-Yong Kim Yeongeun Kim Sukyoung Choi Ki-Jung Paeng |
| author_sort | Taewoo Yum |
| collection | DOAJ |
| description | Fatty acid analysis is an essential step in evaluating the potential of macroalgae for biodiesel production. An extraction method was developed to simultaneously analyze up to five types of biodiesel-fuel-related fatty acids (myristic acid, palmitic acid, <i>cis</i>-palmitvaccenic acid, stearic acid, and oleic acid) in macroalgae using liquid chromatography and tandem mass spectrometry (LC–MS/MS). Lypophilization and solid-phase extraction (SPE) techniques were applied to improve the extraction efficiency and effectively purify samples. The optimal conditions for SPE were set by comparing the recoveries according to the various solvent conditions for each step (loading, washing, and elution). In addition, the introduction of trimethylaminoethyl (TMAE) derivatives to the hydroxyl group of the target analyte increased the ionization efficiency and sensitivity. The derivatized samples were analyzed using the LC–MS/MS method with electrospray ionization in the positive and multiple-reaction monitoring modes. The target analytes were separated and detected within 13.5 min using a CAPCELL PAK C18 MGII S3 column. Gradient elution was performed using distilled water and acetonitrile containing 5 mM ammonium acetate. This method offers a reliable and sensitive tool for the analysis of macroalgae samples for their potential use in biodiesel production. To the best of our knowledge, this is the first report on the simultaneous determination of fatty acids in macroalgae using LC–MS/MS with TMAE derivatization. |
| first_indexed | 2024-03-08T09:49:37Z |
| format | Article |
| id | doaj.art-58d9939517094ce8bb6b9592d29fd4d2 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-08T09:49:37Z |
| publishDate | 2024-01-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-58d9939517094ce8bb6b9592d29fd4d22024-01-29T14:08:33ZengMDPI AGMolecules1420-30492024-01-0129243010.3390/molecules29020430The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MSTaewoo Yum0Eun-Yong Kim1Yeongeun Kim2Sukyoung Choi3Ki-Jung Paeng4Department of Chemistry, Yonsei University, Wonju 26493, Republic of KoreaDepartment of Chemistry, Yonsei University, Wonju 26493, Republic of KoreaDepartment of Chemistry, Yonsei University, Wonju 26493, Republic of KoreaDepartment of Chemistry, Yonsei University, Wonju 26493, Republic of KoreaDepartment of Chemistry, Yonsei University, Wonju 26493, Republic of KoreaFatty acid analysis is an essential step in evaluating the potential of macroalgae for biodiesel production. An extraction method was developed to simultaneously analyze up to five types of biodiesel-fuel-related fatty acids (myristic acid, palmitic acid, <i>cis</i>-palmitvaccenic acid, stearic acid, and oleic acid) in macroalgae using liquid chromatography and tandem mass spectrometry (LC–MS/MS). Lypophilization and solid-phase extraction (SPE) techniques were applied to improve the extraction efficiency and effectively purify samples. The optimal conditions for SPE were set by comparing the recoveries according to the various solvent conditions for each step (loading, washing, and elution). In addition, the introduction of trimethylaminoethyl (TMAE) derivatives to the hydroxyl group of the target analyte increased the ionization efficiency and sensitivity. The derivatized samples were analyzed using the LC–MS/MS method with electrospray ionization in the positive and multiple-reaction monitoring modes. The target analytes were separated and detected within 13.5 min using a CAPCELL PAK C18 MGII S3 column. Gradient elution was performed using distilled water and acetonitrile containing 5 mM ammonium acetate. This method offers a reliable and sensitive tool for the analysis of macroalgae samples for their potential use in biodiesel production. To the best of our knowledge, this is the first report on the simultaneous determination of fatty acids in macroalgae using LC–MS/MS with TMAE derivatization.https://www.mdpi.com/1420-3049/29/2/430macroalgaefatty acidtrimethylaminoethyl derivativessolid-phase extractionLC–ESI–MS/MS |
| spellingShingle | Taewoo Yum Eun-Yong Kim Yeongeun Kim Sukyoung Choi Ki-Jung Paeng The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS Molecules macroalgae fatty acid trimethylaminoethyl derivatives solid-phase extraction LC–ESI–MS/MS |
| title | The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS |
| title_full | The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS |
| title_fullStr | The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS |
| title_full_unstemmed | The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS |
| title_short | The Development of an Extraction Method for Simultaneously Analyzing Fatty Acids in Macroalgae Using SPE with Derivatization for LC–MS/MS |
| title_sort | development of an extraction method for simultaneously analyzing fatty acids in macroalgae using spe with derivatization for lc ms ms |
| topic | macroalgae fatty acid trimethylaminoethyl derivatives solid-phase extraction LC–ESI–MS/MS |
| url | https://www.mdpi.com/1420-3049/29/2/430 |
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