Method for supercritical separation and purification of 4,8-dht from pecan exocarp

Abstract

The invention discloses a method for supercritical separation and purification of 4.8-DHT from pecan epicarp. The method comprises the following steps: extracting through a supercritical extraction kettle to obtain an extract; absorbing the extract by using methanol; carrying out silicagel column chromatography; carrying out gradient eluting by using a mixed solvent of petroleum ether and ethyl acetate; collecting a bottle of fluid per column volume, collecting 10 bottles of fluid in all; carrying out reduced-pressure concentration on the fourth bottle of fluid; and crystallizing by using ethyl acetate to obtain a 4,8-dyhydroxy-1-tetralone crystal compound. The 4,8-DHT is a 1:1 raceme and low in impurity content; the purity is 99.82%; the extraction rate is over 60%; and the 4.8-DHT raceme has the effects of inhibiting plant seed germination and seedling growth.

Description

technical field

[0001] The invention relates to extraction of 4,8-dihydroxy-1-tetralone, in particular to a method for supercritical separation and purification of 4,8-dihydroxy-1-tetralone from pecan exocarp. Background technique

[0002] 4,8-dihydroxy-1-tetralone (4,8-DHT), chemical name 4,8-dihydroxy-1-tetralone, colorless fine cluster needle crystal, in which the 4th carbon connected to the hydroxyl group is a chiral carbon. The left-handed enantiomer (–) of 4,8-DHT is called regiolone and the right-handed enantiomer (+) is called isosclerone. Regiolone was first identified from green walnut and can be used to treat skin itching and pain. Isosclerone was first introduced from Sclerotinia sclerotium The compound was isolated and identified in , and later also isolated from some fungi, which can cause grape gray spot disease. Pecan exocarp also contains 4,8-DHT, which is a 1:1 racemate, melting point 366-368K, soluble in water, ethanol, acetone and chloroform, [α] 2...