Harald Svensen, Geir Frode Olsen, John-Erik Haugen
{"title":"经验证的GC-FID法测定甘油三酯鱼油中超长链多不饱和脂肪酸(C24-C30 n−3","authors":"Harald Svensen, Geir Frode Olsen, John-Erik Haugen","doi":"10.1002/ejlt.70040","DOIUrl":null,"url":null,"abstract":"<div>\n \n <p>A quantitative and in-house validated gas chromatography–flame ionization detector (GC-FID) method for the analysis of methyl esters of very long chain (C24–C30, 4–8 double bonds) polyunsaturated fatty acids (VLC-PUFAs) in triglyceride (TG) fish oils has been developed. Quantification of VLC-PUFA was obtained by use of empirical response factors relative to the long-chain PUFA DHA. The identification of VLC-PUFA was achieved using GC-positive chemical ionization-mass spectroscopy (PCI-MS) and electron ionization-mass spectroscopy (EI-MS) fragmentation patterns. Method performance parameters have been investigated: Results showed a high linearity (<i>r</i> = 0.999, <i>n</i> = 15, <i>p</i> < 0.001), an overall accuracy/recovery of 98% ± 0.3%, repeatability of 0.8%, and precision of 1.7%. Limit of detection of individual VLC-PUFA was in the range of 0.2 mg/g (<i>S</i>/<i>N</i> = 3). The results have shown that the GC-FID method is applicable for quantifying the levels of individual VLC-PUFA and the total amount of VLC-PUFA levels in TG fish oils in the range of 20–70 mg/g fish oil.</p>\n <p><i>Practical Applications</i>: Our results have shown that it is possible to obtain a routine quantitative determination of the methyl esters of the individual VLC-PUFA in triglyceride fish oils after an initial GC-EI-MS and GC-PCI-MS confirmation of the fatty acid structures. Investigation of method performance parameters has shown that our requirements for linearity, accuracy, repeatability, precision, and limit of quantification and detection have been met. The results show that the GC-FID method is able to quantify the total amount of VLC-PUFA levels in triglyceride fish oils in the range of 20–70 mg/g fish oil. This method may represent a useful tool for determining VLC-PUFA content in commercial fish oil products. The method could also have the potential to be used with other types of lipids, such as ethyl esters, free fatty acids, phospholipids, wax esters, and even extracts of biological samples.</p>\n </div>","PeriodicalId":11988,"journal":{"name":"European Journal of Lipid Science and Technology","volume":"127 8","pages":""},"PeriodicalIF":1.8000,"publicationDate":"2025-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"A Validated GC-FID Method for Determination of Very Long-Chain Polyunsaturated Fatty Acids (C24–C30 n − 3) in Triglyceride Fish Oils\",\"authors\":\"Harald Svensen, Geir Frode Olsen, John-Erik Haugen\",\"doi\":\"10.1002/ejlt.70040\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div>\\n \\n <p>A quantitative and in-house validated gas chromatography–flame ionization detector (GC-FID) method for the analysis of methyl esters of very long chain (C24–C30, 4–8 double bonds) polyunsaturated fatty acids (VLC-PUFAs) in triglyceride (TG) fish oils has been developed. Quantification of VLC-PUFA was obtained by use of empirical response factors relative to the long-chain PUFA DHA. The identification of VLC-PUFA was achieved using GC-positive chemical ionization-mass spectroscopy (PCI-MS) and electron ionization-mass spectroscopy (EI-MS) fragmentation patterns. Method performance parameters have been investigated: Results showed a high linearity (<i>r</i> = 0.999, <i>n</i> = 15, <i>p</i> < 0.001), an overall accuracy/recovery of 98% ± 0.3%, repeatability of 0.8%, and precision of 1.7%. Limit of detection of individual VLC-PUFA was in the range of 0.2 mg/g (<i>S</i>/<i>N</i> = 3). The results have shown that the GC-FID method is applicable for quantifying the levels of individual VLC-PUFA and the total amount of VLC-PUFA levels in TG fish oils in the range of 20–70 mg/g fish oil.</p>\\n <p><i>Practical Applications</i>: Our results have shown that it is possible to obtain a routine quantitative determination of the methyl esters of the individual VLC-PUFA in triglyceride fish oils after an initial GC-EI-MS and GC-PCI-MS confirmation of the fatty acid structures. Investigation of method performance parameters has shown that our requirements for linearity, accuracy, repeatability, precision, and limit of quantification and detection have been met. The results show that the GC-FID method is able to quantify the total amount of VLC-PUFA levels in triglyceride fish oils in the range of 20–70 mg/g fish oil. This method may represent a useful tool for determining VLC-PUFA content in commercial fish oil products. The method could also have the potential to be used with other types of lipids, such as ethyl esters, free fatty acids, phospholipids, wax esters, and even extracts of biological samples.</p>\\n </div>\",\"PeriodicalId\":11988,\"journal\":{\"name\":\"European Journal of Lipid Science and Technology\",\"volume\":\"127 8\",\"pages\":\"\"},\"PeriodicalIF\":1.8000,\"publicationDate\":\"2025-06-18\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"European Journal of Lipid Science and Technology\",\"FirstCategoryId\":\"97\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/ejlt.70040\",\"RegionNum\":3,\"RegionCategory\":\"农林科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"FOOD SCIENCE & TECHNOLOGY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"European Journal of Lipid Science and Technology","FirstCategoryId":"97","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/ejlt.70040","RegionNum":3,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"FOOD SCIENCE & TECHNOLOGY","Score":null,"Total":0}
A Validated GC-FID Method for Determination of Very Long-Chain Polyunsaturated Fatty Acids (C24–C30 n − 3) in Triglyceride Fish Oils
A quantitative and in-house validated gas chromatography–flame ionization detector (GC-FID) method for the analysis of methyl esters of very long chain (C24–C30, 4–8 double bonds) polyunsaturated fatty acids (VLC-PUFAs) in triglyceride (TG) fish oils has been developed. Quantification of VLC-PUFA was obtained by use of empirical response factors relative to the long-chain PUFA DHA. The identification of VLC-PUFA was achieved using GC-positive chemical ionization-mass spectroscopy (PCI-MS) and electron ionization-mass spectroscopy (EI-MS) fragmentation patterns. Method performance parameters have been investigated: Results showed a high linearity (r = 0.999, n = 15, p < 0.001), an overall accuracy/recovery of 98% ± 0.3%, repeatability of 0.8%, and precision of 1.7%. Limit of detection of individual VLC-PUFA was in the range of 0.2 mg/g (S/N = 3). The results have shown that the GC-FID method is applicable for quantifying the levels of individual VLC-PUFA and the total amount of VLC-PUFA levels in TG fish oils in the range of 20–70 mg/g fish oil.
Practical Applications: Our results have shown that it is possible to obtain a routine quantitative determination of the methyl esters of the individual VLC-PUFA in triglyceride fish oils after an initial GC-EI-MS and GC-PCI-MS confirmation of the fatty acid structures. Investigation of method performance parameters has shown that our requirements for linearity, accuracy, repeatability, precision, and limit of quantification and detection have been met. The results show that the GC-FID method is able to quantify the total amount of VLC-PUFA levels in triglyceride fish oils in the range of 20–70 mg/g fish oil. This method may represent a useful tool for determining VLC-PUFA content in commercial fish oil products. The method could also have the potential to be used with other types of lipids, such as ethyl esters, free fatty acids, phospholipids, wax esters, and even extracts of biological samples.
期刊介绍：
The European Journal of Lipid Science and Technology is a peer-reviewed journal publishing original research articles, reviews, and other contributions on lipid related topics in food science and technology, biomedical science including clinical and pre-clinical research, nutrition, animal science, plant and microbial lipids, (bio)chemistry, oleochemistry, biotechnology, processing, physical chemistry, and analytics including lipidomics. A major focus of the journal is the synthesis of health related topics with applied aspects.
Following is a selection of subject areas which are of special interest to EJLST:
Animal and plant products for healthier foods including strategic feeding and transgenic crops
Authentication and analysis of foods for ensuring food quality and safety
Bioavailability of PUFA and other nutrients
Dietary lipids and minor compounds, their specific roles in food products and in nutrition
Food technology and processing for safer and healthier products
Functional foods and nutraceuticals
Lipidomics
Lipid structuring and formulations
Oleochemistry, lipid-derived polymers and biomaterials
Processes using lipid-modifying enzymes
The scope is not restricted to these areas. Submissions on topics at the interface of basic research and applications are strongly encouraged. The journal is the official organ the European Federation for the Science and Technology of Lipids (Euro Fed Lipid).
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