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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
Journal of Agricultural and Food Chemistry ( IF 6.1 ) Pub Date : 2018-12-07 00:00:00 , DOI: 10.1021/acs.jafc.8b05462
David T. Mannion 1, 2 , Ambrose Furey 2 , Kieran N. Kilcawley 1
Affiliation  

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; R2 > 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.

中文翻译:

测定乳制品中游离脂肪酸的新型游离脂肪酸丁基酯气相色谱法的开发与验证

乳制品中游离脂肪酸的准确定量对于产品质量控制和立法目的都很重要。在这项研究中,开发了一种新的脂肪酸丁酯方法,该方法将提取的游离脂肪酸转化为丁酯,然后进行气相色谱和火焰离子化检测。该方法经过全面验证,可建立线性关系(20–700 mg / L;R 2> 0.9964),检出限(5–8 mg / L),定量限(15–20 mg / L),准确度(1.6–5.4%相对误差),日间精确度(4.4–5.3%相对标准偏差),每种游离脂肪酸的日内精确度(相对标准偏差为0.9-5.6%)。共分析了17个乳制品样品,涵盖了各种样品基质,脂肪含量和脂解程度。将该方法与直接柱上注射法和脂肪酸甲酯法进行了比较,并克服了与这些方法相关的局限性,例如柱相吸收或降解,短链游离脂肪酸的准确定量以及对多不饱和游离脂肪的低估酸。
更新日期:2018-12-07
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