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Development and Validation of a Novel Free Fatty Acid Butyl Ester Gas Chromatography Method for the Determination of Free Fatty Acids in Dairy Products

机译:新型游离脂肪酸丁酯气相色谱法测定乳制品中游离脂肪酸的开发和验证

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摘要

Accurate quantification of free fatty acids in dairy products is important for both product quality control and legislative purposes. In this study, a novel fatty acid butyl ester method was developed, where extracted free fatty acids are converted to butyl esters prior to gas chromatography with flame ionization detection. The method was comprehensively validated to establish linearity (20-700 mg/L; R-2 0.9964), limits of detection (5-8 mg/L), limits of quantification (15-20 mg/L), accuracy (1.6-5.4% relative error), interday precision (4.4-5.3% relative standard deviation), and intraday precision (0.9-5.6% relative standard deviation) for each individual free fatty acid. A total of 17 dairy samples were analyzed, covering diverse sample matrices, fat content, and degrees of lipolysis. The method was compared to direct on-column injection and fatty acid methyl ester methods and overcomes limitations associated with these methods, such as either column-phase absorption or deterioration, accurate quantification of short-chain free fatty acids, and underestimation of polyunsaturated free fatty acid.
机译:准确定量乳制品的游离脂肪酸对于产品质量控制和立法目的很重要。在该研究中,开发了一种新型脂肪酸丁酯方法,其中萃取的游离脂肪酸在与火焰电离检测中的气相色谱之前转化为丁基酯。该方法全面验证以建立线性度(20-700mg / L; r-2> 0.9964),检测限制(5-8 mg / L),量化限制(15-20 mg / L),精度( 1.6-5.4%的相对误差),中间精度(相对标准偏差4.4-5.3%),以及每个单独的游离脂肪酸的盘区精度(相对标准偏差0.9-5.6%)。分析了17种乳制品样本,覆盖了不同的样品基质,脂肪含量和脂肪分解程度。将该方法与直接柱注射和脂肪酸甲酯方法进行比较,克服与这些方法相关的限制,例如柱相吸收或劣化,准确定量短链游离脂肪酸,并低估多不饱和无脂肪脂肪酸。

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