Comprehensive comparison of fatty acid methyl ester profile in different food matrices using microwave-assisted extraction and derivatization methods and comprehensive two-dimensional gas chromatography coupled with flame ionization detection

IF 5.2 Q1 CHEMISTRY, ANALYTICAL Advances in Sample Preparation Pub Date : 2024-08-01 DOI:10.1016/j.sampre.2024.100124
Donatella Ferrara , Marco Beccaria , Chiara E. Cordero , Giorgia Purcaro
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Abstract

Analyzing fatty acids provides key insights into fat composition for industrial applications and their implications for nutrition and health. Typically, fatty acid analysis involves extracting lipids from the matrix and converting them into fatty acid methyl esters (FAME) through a derivatization process before gas chromatography (GC) analysis. Either one-step or two-step procedures can be found in the literature and as official methods. In this work, different methods exploiting microwave-assisted processes were compared with two official methods from the American Oil Chemical Society (AOCS). Especially, two types of microwave-assisted extractions were employed: solvent extraction and extraction with hydrolysis. The extracts were derivatized using either BF3 or a microwave-assisted methanolic hydrogen chloride solution. These combinations of extraction and derivatization methods were compared also with one-step microwave-assisted extraction and derivatization, and two AOCS reference methods, resulting in seven different methods applied to six different food matrices. The performance of the different procedures was compared based on the FAME profile obtained from the comprehensive two-dimensional GC (GC × GC)-FID analysis.

Microwave-assisted processes were shown to be effective, yielding results comparable to the official methods in both the one-step and two-step methods. Moreover, it was shown that the BF3 derivatization could be safely replaced with microwave-assisted derivatization with methanolic hydrogen chloride, providing equivalent performances while enhancing operator safety and environmental friendliness. Some discrepancies in the FAMEs profile were highlighted for the sample of oats, the only explicitly requiring acidic hydrolysis for lipid extraction. Further studies are required to understand the reasons behind these differences and develop a suitable modified method. In conclusion, all the methods were evaluated for greenness and blueness with two specific tools: AGREEprep and BAGI.

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利用微波辅助萃取和衍生化方法以及二维气相色谱-火焰离子化检测法全面比较不同食品基质中脂肪酸甲酯的概况
分析脂肪酸可以深入了解工业应用中的脂肪成分及其对营养和健康的影响。通常情况下,脂肪酸分析包括从基质中提取脂类,并在气相色谱 (GC) 分析之前通过衍生化过程将其转化为脂肪酸甲酯 (FAME)。一步法或两步法均可在文献和官方方法中找到。在这项工作中,利用微波辅助工艺的不同方法与美国石油化学学会(AOCS)的两种官方方法进行了比较。特别是采用了两种微波辅助萃取法:溶剂萃取和水解萃取。萃取物使用 BF3 或微波辅助甲醇氯化氢溶液进行衍生。将这些萃取和衍生方法的组合与一步式微波辅助萃取和衍生方法以及两种 AOCS 参考方法进行了比较,得出了适用于六种不同食品基质的七种不同方法。根据二维气相色谱(GC × GC)- FID 综合分析所得到的 FAME 图谱,对不同方法的性能进行了比较。结果表明,微波辅助方法是有效的,无论是一步法还是两步法,其结果都与官方方法相当。此外,研究还表明可以用甲醇氯化氢微波辅助衍生法安全地取代 BF3 衍生法,在提高操作安全性和环境友好性的同时提供同等的性能。燕麦样品的 FAMEs 图谱存在一些差异,这是唯一明确需要酸性水解提取脂质的样品。需要进一步研究以了解这些差异背后的原因,并开发出合适的改进方法。总之,所有方法都使用两种特定工具对绿色度和蓝色度进行了评估:AGREEprep 和 BAGI。
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