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Method for separating and purifying 4,8-dht from pecan exocarp and application of 4,8-dht

A technology for separation and purification of 8-DHT, applied in the field of 4,8-DHT application, separation and purification of 4,8-dihydroxy-1-tetralone, to achieve the effect of inhibiting plant seed germination, inhibiting seedling growth, and less impurities Effect

Active Publication Date: 2016-05-25
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

[0013] The method of separating and purifying 4,8-DHT from the pecan exocarp, crushing the air-dried pecan exocarp, passing through a 45-60 mesh sieve to obtain 10g of hickory exocarp powder, and putting the hickory exocarp powder into ultrasonic extraction Add 180-200ml of distilled water to the kettle, and the method of ultrasonic generation is: it excites the ultrasonic sound, radially vibrates the columnar transducer, the ultrasonic power is 100W, the ultrasonic frequency is 28kHz, and the extraction method is ultrasonic once every 2min, each time 4min , under the condition of air-lift stirring at 25°C, ultrasonically extract for 30-45min, filter to obtain the extract of pecan exocarp; under the condition of pressure of 450-500Pa, the extract of pecan exocarp is concentrated under reduced pressure to the original volume 1 / 10, and then passed through X-5 macroporous resin, with volume ratios of 10:0, 9:1, 8:2, 7:3, 6:4, 5:5, 4:6, 3:7 , 2:8, 1:9, 0:10 mixed solution of water...

Embodiment 2

[0015] The 4,8-dihydroxyl-1-tetralone of Example 1 is configured into 0.1mM, 0.5mM treatment solution for the germination inhibition experiment of lettuce, radish, cucumber, onion, wheat seeds, and each 100 seeds of the test species are taken , placed evenly in a germination box with two layers of filter paper, the size is 15×20cm, and 10ml of different concentrations of treatment solutions were added (the control group was deionized water), and each treatment set 3 replicates. The culture conditions were light cycle 25°C, 12h; dark cycle 15°C, 12h. Seed germination is based on the radicle breaking through the seed coat. The number of lettuce seeds germinated on the fourth and seventh days, the number of radish seeds germinated on the fourth and tenth days, and the cucumber seeds and wheat seeds on the fourth and eighth days The number of germination, the number of germination of onion seeds was recorded on the sixth day and the twelfth day. The final result: 0.1mM 4,8-DHT tr...

Embodiment 3

[0017] The 4,8-dihydroxy-1-tetralone of Example 1 is configured into 0.1mM, 0.5mM treatment solution for the inhibition experiment on the growth of lettuce, radish, cucumber, onion, wheat seedlings, and the radicle is taken to break through the seed coat 100 seeds of each seed were evenly placed in a germination box with a size of 15 × 20 cm covered with two layers of filter paper, and 10 ml of different concentrations of treatment solutions were added (the control group was deionized water), and three replicates were set for each treatment. The culture conditions were light cycle 25°C, 12h; dark cycle 15°C, 12h. Every other day, 5 seeds were randomly selected from the germination box to measure the length of radicle, germ and fresh weight, and the measurements were taken 6 times in total. 0.1mM and 0.5mM4,8-DHT treatment can significantly reduce the radicle growth of test species (p<0.05). 0.1mM 4,8-DHT treatment can inhibit the growth of lettuce germ by about 45%, the growt...

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Abstract

The invention discloses a method for separating and purifying 4,8-DHT from pecan exocarp and an application of 4,8-DHT. The method comprises the following steps: performing ultrasonic extraction to obtain a pecan exocarp extracting liquid by virtue of independent excitation type ultrasonic sounding, performing reduced pressure concentration, then passing through X-5 macroporous resin, performing gradient elution by using a mixed solution of water and ethanol, collecting an eluate obtained by eluting with a mixed liquid of water and ethanol in a volume ratio of 4 to 6, performing reduced pressure concentration to obtain a concentrated solution, performing silica-gel column chromatography, performing gradient elution by using a mixed solvent of petroleum ether and ethyl acetate, totally collecting 36 bottles of flow components by collecting a bottle of the flow components per 1 / 2 column volume, combining the tenth to eighteenth bottles of the flow components, performing reduced pressure concentration, and performing ethyl acetate crystallization to obtain a 4,8-dyhydroxy-1-tetralone crystalline compound. 4,8-DHT disclosed by the invention is of a 1:1 raceme, is less in impurity, has the purity of 99.5-99.8%, and ensures that the extraction rate reaches more than 94%; and the 4,8-DHT raceme has the effects on inhibiting seed germination and seedling growth of plants.

Description

technical field [0001] The invention relates to the extraction of 4,8-dihydroxy-1-tetralone, in particular to a method for separating and purifying 4,8-dihydroxy-1-tetralone from the exocarp of hickory nut and the application of 4,8-DHT . 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, ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/747C07C45/78A01P21/00
CPCA01N35/06C07C45/78C07C45/79C07C2602/28C07C49/747
Inventor 王强
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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