食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
Journal of Food Safety & Quality
2015年
10期
4103-4109
,共7页
张星星%胡志雄%贺军波%张维农%齐玉堂
張星星%鬍誌雄%賀軍波%張維農%齊玉堂
장성성%호지웅%하군파%장유농%제옥당
月桂酸缩水甘油酯%合成%纯化%表征
月桂痠縮水甘油酯%閤成%純化%錶徵
월계산축수감유지%합성%순화%표정
glycidyl laurate%synthesis%purification%characterization
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。
目的:研究月桂痠縮水甘油酯的有效閤成、純化方法,為食用油脂中脂肪痠縮水甘油酯的檢測提供相關對照品。方法以月桂痠鈉和環氧氯丙烷為起始原料,四丁基溴化銨為催化劑,採用相轉催化法一步閤成瞭月桂痠縮水甘油酯,通過甲醇/正己烷為萃取溶液及重結晶的方式得到純品。純化後的產物經高效液相、紅外光譜、元素分析、質譜等手段進行錶徵。結果產物經錶徵後確證為月桂痠縮水甘油酯,在優化條件下產物的純度可達95%以上,符閤標準對照品的純度要求。結論該方法以環氧氯丙烷為反應物和溶劑,原料易得、成本低廉,反應效率高、操作簡便,為脂肪痠縮水甘油酯的閤成提供瞭一種有效途徑與方法。
목적:연구월계산축수감유지적유효합성、순화방법,위식용유지중지방산축수감유지적검측제공상관대조품。방법이월계산납화배양록병완위기시원료,사정기추화안위최화제,채용상전최화법일보합성료월계산축수감유지,통과갑순/정기완위췌취용액급중결정적방식득도순품。순화후적산물경고효액상、홍외광보、원소분석、질보등수단진행표정。결과산물경표정후학증위월계산축수감유지,재우화조건하산물적순도가체95%이상,부합표준대조품적순도요구。결론해방법이배양록병완위반응물화용제,원료역득、성본저렴,반응효솔고、조작간편,위지방산축수감유지적합성제공료일충유효도경여방법。
ObjectiveTo 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. MethodsGlycidyl 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). ResultsThe 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 would guarantee many advantages such as easily obtaining of raw materials, low cost,high efficiency and simple operation. Therefore, the proposed method would provide an effective approach for the synthesis of glycidyl fatty acid ester.