A Validated GC-FID Method for Determination of Very Long-Chain Polyunsaturated Fatty Acids (C24–C30 n − 3) in Triglyceride Fish Oils

IF 1.8 3区农林科学 Q3 FOOD SCIENCE & TECHNOLOGY

European Journal of Lipid Science and Technology Pub Date : 2025-06-18 DOI:10.1002/ejlt.70040

Harald Svensen, Geir Frode Olsen, John-Erik Haugen

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引用次数: 0

Abstract

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.

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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

建立了一种用于分析甘油三酯（TG）鱼油中超长链（C24-C30, 4-8双键）多不饱和脂肪酸（VLC-PUFAs）甲酯的定量和内部验证的气相色谱火焰电离检测器（GC-FID）方法。VLC-PUFA的定量是通过使用与长链PUFA DHA相关的经验响应因子得到的。采用气相色谱阳性化学电离-质谱（PCI-MS）和电子电离-质谱（EI-MS）破碎图谱对VLC-PUFA进行鉴定。考察了方法的性能参数：结果表明：线性关系良好(r = 0.999, n = 15, p <；0.001)，总体准确度/回收率为98%±0.3%，重复性为0.8%，精密度为1.7%。单个VLC-PUFA的检出限在0.2 mg/g范围内（S/N = 3）。结果表明，气相色谱- fid法适用于20 ~ 70 mg/g TG鱼油中单个VLC-PUFA含量和VLC-PUFA总量的定量分析。实际应用：我们的结果表明，在对脂肪酸结构进行初始GC-EI-MS和GC-PCI-MS确认后，可以对甘油三酯鱼油中单个VLC-PUFA的甲酯进行常规定量测定。对方法性能参数的研究表明，该方法在线性度、准确度、重复性、精密度、定量检出限等方面均满足要求。结果表明，气相色谱- fid方法能够定量测定甘油三酯鱼油中VLC-PUFA含量在20 ~ 70 mg/g范围内的总量。该方法可作为测定商业鱼油产品中VLC-PUFA含量的有效工具。该方法也有可能用于其他类型的脂类，如乙酯、游离脂肪酸、磷脂、蜡酯，甚至生物样品的提取物。

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来源期刊

European Journal of Lipid Science and Technology 工程技术-食品科技

CiteScore

5.50

自引率

0.00%

发文量

101

审稿时长

6-16 weeks

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).