山核桃叶球松素制备工艺研究

Study on Preparation Process of Pinostrobin from the Leaves of Carya Cathayensis Sarg.

关键词:  山核桃叶  球松素  制备工艺  聚酰胺  氢氧化钠

Key words:  Carya cathayensis Sarg.  pinostrobin  preparation process  polyamide resin  sodium hydroxide

摘要:

目的 优化山核桃叶球松素的制备工艺，为进一步开发利用山核桃叶提供理论依据。方法 采用单因素试验，山核桃叶通过乙醇回流提取，氢氧化钠变性，聚酰胺吸附并洗脱，石油醚萃取，乙醇结晶等步骤，以球松素作为检测指标，进行RP-HPLC测定。结果 山核桃叶球松素的制备工艺为山核桃叶粉末用10倍量的95%乙醇回流提取2次，每次30 min，以体积比400：5的比例往提取液中加入1 mol·L^-1氢氧化钠溶液，静置过夜取上清，以液质比20：1的比例与聚酰胺混合并旋蒸至干燥，先用15倍量聚酰胺体积的水洗去杂质，再用15倍量聚酰胺体积的20%乙醇溶液洗去杂质，最后用15倍量聚酰胺体积的60%乙醇溶液解吸附；收集60%乙醇溶液洗脱液，浓缩至干后，获得球松素含量在20%左右的粗产物，以液质比50：3的比例将此粗产物溶解于甲醇溶液中，加入等体积石油醚，连续萃取10次，收集石油醚产物，再将此产物用乙醇进行结晶，获得纯度>90%的球松素。结论 该方法稳定可行，适合工业生产；氢氧化钠变性、聚酰胺纯化及结晶是制备高纯度球松素的关键步骤，为球松素大规模制备奠定了基础，也为山核桃叶的开发利用提供了理论依据。

Abstract:

OBJECTIVE To optimize the preparation process of pinostrobin from the leaves of Carya cathayensis Sarg. and to provide theoretical basis for further development and utilization of the leaves. METHODS Signal factor test was investigated to optimize the manufacturing process of pinostrobin. Pinostrobin was obtained by alcohol-backflow extracting, sodium hydroxide degeneration, adsorption and desorption of polyamide resins, extract of petroleum ether, alcohol crystallization and determined by RP-HPLC. RESULTS The best preparation process of pinostrobin was as follows:the powdered leaves were extracted twice with 95% ethanol by reflux for 30 min at 100℃. Add 1 mol·L^-1 sodium hydroxide solution to the extraction solution with a volume ratio of 400:5, then let it rest the night and take the supernatant mixed with polyamide and rotate to dry with liquid ratio 20:1. The sample-laden polyamide resins were added to a glass column and first washed with 15 BV deionized water, second with 15 BV 20% ethanol-water solution and last with 15 BV 60% ethanol-water solution which was concentrated and dried. Crude from 60% ethanol-water solution was dissolved in methanol and extracted 10 times continuously with petroleum ether. The product from petroleum ether was dissolved and crystallized in ethanol-water solution and the pinostrobin with high purity (> 90%) was obtained. CONCLUSION The method is stable and feasible, and is suitable for industrial production. Sodium hydroxide degeneration, adsorption and desorption of polyamide resins and alcohol crystallization are the key steps to obtain high purity pinostrobin which can lay the foundation for pinostrobin preparation at large scale, also provides theoretical basis for the development and utilization of the leaves.