지방산 분석을 위한 trimethylsulphonium hydroxide (TMSH) 조건 확립

Study on trimethylsulphonium hydroxide (TMSH) for fatty acid analysis

This study was carried out to develop a simple and rapid methylation method for fatty acids in fish oils which contain lots of polyunsaturated fatty acids. Methanolic rimethylsulfonium hydroxide (0.2 M in methanol, TMSH) was preprepared by trimethylsulfonium iodide (0.40 g, TMSI), 0.88g of silver oxide, and 10 mL anhydrous methanol in the test tube. The mixture allowed to react for several hours. If a positive iodide test resulted the agitation, centrifugation and testing procedure were prepeated until no iodide could be detected in the reagent solution. Generally the reaction was completed within two hours at room temperature. The transesterification of fatty acid of a squid oil was monitored with thin layer chromatography (TLC) by spot the mixture of the 250 μL of TMSH reagent and 500 μL sample oil (20 ㎎/mL). Usually the transesterification was occurred from 2 minutes and the reaction was completed in 14 minutes. The TMSH reagent compared with the commercial Prep Ⅱ esterification reagent. The time of methylation reaction was similar between the TMSH and Prep Ⅱ. For full reaction of transesterification, twenty minutes were recommended. The fatty acid content of squid oil obtained by transesterification was the highest in the 15 minutes of reaction. However, the contents was decreased at 20 minutes reaction. The methylation with TMSH showed a simple and rapid method for fish oil.