月桂酸缩水甘油酯的相转移催化合成与表征

目的研究月桂酸缩水甘油酯的有效合成、纯化方法,为食用油脂中脂肪酸缩水甘油酯的检测提供相关对照品。方法以月桂酸钠和环氧氯丙烷为起始原料,四丁基溴化铵为催化剂,采用相转催化法一步合成了月桂酸缩水甘油酯,通过甲醇/正己烷为萃取溶液及重结晶的方式得到纯品。纯化后的产物经高效液相、红外光谱、元素分析、质谱等手段进行表征。结果产物经表征后确证为月桂酸缩水甘油酯,在优化条件下产物的纯度可达95%以上,符合标准对照品的纯度要求。结论该方法以环氧氯丙烷为反应物和溶剂,原料易得、成本低廉,反应效率高、操作简便,为脂肪酸缩水甘油酯的合成提供了一种有效途径与方法。

Phase transfer catalytic synthesis and characterization of glycidyl laurate

Objective To study the effective synthesis and purification methods of glycidyl laurate and provide standard reference products for the detection of glycidyl fatty acid ester in edible oils and fats. Methods In this paper, glycidyl laurate has been synthesized by one-step phase transfer catalysis with sodium laurate (SL) and epichlorohydrin (ECH) as reactants and tetrabutyl ammonium bromide (TBAB) as catalyst, the resultant products were purified by liquid-liquid extraction with the mixture solvent of methanol and hexane, the residue of hexane layer was then recrystallized to prepare purified samples. The obtained products were characterized by high performance liquid chromatography (HPLC), infrared spectrum (IR), elemental analysis and mass spectrum (MS). Results The product was confirmed to be glycidyl laurate, and its purity could reach more than 95% under optimized conditions, which conformed to the required purity of standard reference material. Conclusion Epichlorohydrin was used as reactants and solvents in the phase transfer catalytic synthesis of glycidyl laurate, which will guarantee many advantages such as easily obtaining of raw materials, low cost, high efficiency and simple operation. Therefore, the proposed method will provide an effective approach for the synthesis of glycidyl fatty acid ester.