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

A supercritical separation and 8-DHT technology, applied in the separation/purification of carbonyl compounds, organic chemistry, bulk chemical production, etc., to achieve the effect of inhibiting seedling growth, inhibiting plant seed germination, and reducing impurities

Active Publication Date: 2016-08-24
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is no report on the separation and purification of 4,8-dihydroxy-1-tetralone from the exocarp of hickory nut

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] A method for extracting 4,8-dihydroxy-1-tetralone from the exocarp of hickory nuts. First, the exocarp of hickory nuts air-dried is crushed, passed through a 45-mesh sieve as raw material, weighed 100g, and packed into a supernatant In the critical extraction tank; the extraction temperature is 25°C, CO 2 The fluid pressure is 30MPa, the entrainer ethanol flow rate is 0.15 ml / min, and the extraction time is 2 h; the extract is absorbed with about 25-ml methanol as the absorption liquid, and the absorption liquid is chromatographed on a 200-300 mesh silica gel column, petroleum ether and ethyl acetate Mixed solvent (2:1, 1:1) gradient elution, 2:1 petroleum ether and ethyl acetate mixed solvent, 1:1 petroleum ether and ethyl acetate mixed solvent are used in 5 column bed volumes, flow rate 5mL / min , collected one bottle per column volume, collected 10 fractions in total, concentrated the fourth fraction under reduced pressure, and recrystallized the residue from ethyl ac...

Embodiment 2

[0013] It is basically the same as Example 1, except that the extraction temperature is 30°C, CO 2 The fluid pressure is 20 MPa, the entrainer ethanol flow rate is 0.20 ml / min, and 23.7 mg of small colorless crystals.

Embodiment 3

[0015] Basically the same as Example 1, the only difference is that the extraction temperature is 35 ° C, CO 2 The fluid pressure is 40MPa, the entrainer ethanol flow rate is 0.25 ml / min, and there are 24.9 mg of small colorless crystals.

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PUM

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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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/747C07C45/78A01P21/00
CPCC07C45/79C07C45/80C07C45/81C07C2602/10C07C49/747Y02P20/54
Inventor 王强
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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