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气相色谱-银离子柱对反式脂肪酸的新型预分离方法

Novel pre-fractionation method of trans fatty acids by gas chromatography with silver-ion cartridge column.

作者信息

Goto Hirofumi, Shionoya Noriko, Sugie Megumi, Tominaga Makoto, Shimelis Olga, Taniguchi Makoto, Igarashi Tomoji, Hirata Yoshiaki

机构信息

Japan Food Research Laboratories, Nagoya Branch.

出版信息

J Oleo Sci. 2012;61(2):49-56. doi: 10.5650/jos.61.49.

Abstract

We developed a novel pre-separation method of trans fatty acids (TFAs) using a silver-ion cartridge column and GC. As a preliminary study, a mixture of fatty acid methyl esters consisting of saturated, cis-unsaturated, and trans-unsaturated fatty acids was dissolved in dichloromethane and loaded onto a Bond Elut SCX ion-exchange cartridge column that was converted to the silver-ion form. The column was then eluted with dichloromethane to obtain the saturated fatty acids, dichloromethane/ethyl acetate (90/10) for the trans mono-ene, dichloromethane/ethyl acetate (65/35) for the cis mono-ene, dichloromethane/acetone (60/40) for the trans di-ene, and acetone/acetonitrile (80/20) for the others. Satisfactory separation of the cis/trans isomers was confirmed by GC analysis. To generalize this technique, the elution conditions of the ready-to-use Discovery Ag-ION SPE cartridge column were also optimized. Both cartridge columns had good separation, recovery, and repeatability. Peer laboratory verification was carried out between two laboratories using different production lots of the ready-to-use cartridge column, and the robustness of the product and reproducibility of the method were found to be satisfactory. This technique is therefore a powerful tool not only for routine analyses of TFAs in oils, fats, and foods but also for detailed analyses of TFAs in various research fields.

摘要

我们开发了一种使用银离子柱和气相色谱法(GC)对反式脂肪酸(TFA)进行预分离的新方法。作为一项初步研究,将由饱和、顺式不饱和及反式不饱和脂肪酸组成的脂肪酸甲酯混合物溶解于二氯甲烷中,并加载到转化为银离子形式的Bond Elut SCX离子交换柱上。然后用二氯甲烷洗脱该柱以获得饱和脂肪酸,用二氯甲烷/乙酸乙酯(90/10)洗脱反式单烯,用二氯甲烷/乙酸乙酯(65/35)洗脱顺式单烯,用二氯甲烷/丙酮(60/40)洗脱反式二烯,用丙酮/乙腈(80/20)洗脱其他成分。通过气相色谱分析证实了顺式/反式异构体的良好分离效果。为了推广该技术,还对即用型Discovery Ag-ION固相萃取柱的洗脱条件进行了优化。两种柱均具有良好的分离度、回收率和重复性。使用不同生产批次的即用型柱在两个实验室之间进行了同行实验室验证,发现该产品的稳健性和方法的重现性令人满意。因此,该技术不仅是用于油脂和食品中TFA常规分析的有力工具,也是用于各个研究领域中TFA详细分析的有力工具。

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