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Improved gas chromatography-flame ionization detector analytical method for the analysis of epoxy fatty acids

机译:改进的气相色谱-火焰电离检测器分析环氧脂肪酸的方法

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In this study an improved method for analysis of epoxy fatty acids is reported. Data obtained from analysis of polar fatty acids has previously been presented, but due to the high number of compounds that co-elute in the polar fraction, the resultant chromatograms are complex which may lead to compromising the accuracy of the data. A three steps separation of fatty acid methyl esters (FAMEs) by solid-phase extraction (SPE) on a silica gel column to remove hydroxy fatty acid interferences was proposed. This approach is opposed to a two step separation procedure that has been often used to prevent analytical interferences caused by non-altered fatty acids. A gas chromatograph with a flame ionization detector (GC-FID) equipped with a polar CP-Sil 88? column was used. Quantification was based on the use of methyl nonadecanoate (C19:0), as an internal standard. Individual mono epoxy fatty acids were well separated without co-eluting compounds. The optimized method was finally applied to screen epoxy fatty acids in 37 fresh oil samples. Results obtained for the total epoxy fatty acids were in the range 0.03-2mgg~(-1) of oil with repeatability coefficient of variation (CV) ranging from 2.8 to 9.9% for duplicate analysis showing that the results obtained are repeatable.
机译:在这项研究中,报告了一种改进的分析环氧脂肪酸的方法。先前已经提供了通过极性脂肪酸分析获得的数据,但是由于在极性级分中共洗脱的化合物数量很高,因此所得到的色谱图很复杂,可能会损害数据的准确性。提出了在硅胶柱上通过固相萃取(SPE)分离脂肪酸甲酯(FAME)的三步操作,以消除羟基脂肪酸干扰。该方法与两步分离程序相反,该程序通常用于防止由未改变的脂肪酸引起的分析干扰。配有火焰电离检测器(GC-FID)的气相色谱仪,配有极性CP-Sil 88?使用了列。定量基于壬二酸甲酯(C19:0)作为内标的使用。单独的单环氧脂肪酸可以很好地分离,而无需共洗脱化合物。该优化方法最终应用于筛查37个新鲜油样品中的环氧脂肪酸。获得的全部环氧脂肪酸的结果在油的0.03-2mgg(-1)范围内,重复性变异系数(CV)在2.8%至9.9%之间,重复分析表明结果可重复。

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