文献类型：期刊文献

中文题名：银杏叶聚戊烯醇的分离纯化及其亲水衍生物的合成

英文题名：Separation,Purification and Hydrophilic Derivative Synthesis of Ginkgo biloba Leaves Polyprenol

作者：张昌伟[1] 马余璐[1] 陶冉[1] 叶建中[1] 王成章[1,2]

第一作者：张昌伟

机构：[1]中国林业科学研究院林产化学工业研究所生物质化学利用国家工程实验室国家林业局林产化学工程重点开放性实验室江苏省生物质能源和材料重点实验室;[2]中国林业科学研究院林业新技术研究所

年份：2019

卷号：39

期号：1

起止页码：41-45

中文期刊名：林产化学与工业

外文期刊名：Chemistry and Industry of Forest Products

收录：CSTPCD;;Scopus;北大核心:【北大核心2017】；CSCD:【CSCD2019_2020】；

基金：江苏省生物质能源与材料重点实验室项目(JSBEM-S-201708);江苏省青年基金(SBK2018040639)

语种：中文

中文关键词：聚戊烯醇;分离;纯化;亲水改性

外文关键词：polyprenol;separation;purification;hydrophilic modification

分类号：TQ35

摘要：首先对银杏叶聚戊烯醇含量测定的方法及方法学进行了考察,结果表明:采用高效液相色谱,以C18为色谱柱,以异丙醇/甲醇(体积比32∶18)为流动相,在210 nm下测定聚戊烯醇具有较高的精密度(RSD为0.89%)、较好的稳定性(RSD为3.26%),平均加标回收率为97.4%(RSD为1.75%)。然后通过正己烷提取、皂化、乙醇和丙酮脱蜡,以及硅胶柱层析(V(乙醚)∶V(正己烷)=3∶97)获得纯度为98.6%的聚戊烯醇。在此基础上,对高纯度聚戊烯醇末端羟基进行亲水改性,先与邻苯二甲酰亚胺进行光延反应(mitsunobu反应),再与水合肼进行还原反应,合成了氨基聚戊烯醇,并通过红外和核磁共振氢谱对其结构进行了表征,确认了氨基聚戊烯醇的成功合成。
The analytical methodology and method performance for the determination of polyprenol in Ginkgo biloba leaves were investigated for the first time.The results showed that of the high performance liquid chromatography with C18 as chromatographic column,isopropanol methanol(volume ratio,32∶18)as mobile phase,210 nm as detection wavelength showed high precision(RSD=0.89%)and good stability(RSD=3.26%).In addition,the average standard recovery and RSD value of polyprenol were 97.4%and 1.75%,respectively.Then,polyprenol with the purity of 98.6%was obtained by extraction with n-hexane,saponification,de-waxing with ethanol and acetone,and silica gel column chromatography(V(diethyl ether)∶V(n-hexane)=3∶97).On this basis,the terminal hydroxyl group of high-purity polyprenol was modified to synthesize aminopolyprenol.Firstly,by mitsunobu reaction with phthalimide,followed by reduction reaction with hydrazine hydrate,to obtain aminopolyprenol.The structure of amino polyprenol was characterized by infrared and nuclear magnetic resonance spectroscopy,which confirmed the aminopolyprenol was successfully synthesized.