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.