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The preparation method of r, s-Gaoyichun

A technology of ethyl acetate and extract, which is applied in the field of R, can solve the problems of low purity, low sample yield, and reduced activity of R, S-Caoyichun, etc., to achieve a large amount of single preparation, avoid sample loss, The effect of retaining biological activity

Active Publication Date: 2019-03-29
UNO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method for preparing R, S-Gaoyichun basically adopts macroporous resin column separation, and mostly uses the method of macroporous resin column separation chromatography, normal phase column chromatography and reverse phase column chromatography, but adopts this The sample prepared by the method has low yield, small amount of preparation, and low purity, so it cannot be prepared on a large scale
In addition, this method also has the disadvantages of high pollution, long time consumption and high cost, and the original biological activity of the sample is greatly reduced due to the use of a large amount of adsorption fillers in the preparation process, and the activity of the obtained R,S-Gaoyichun is reduced. Low production efficiency, not suitable for popularization

Method used

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  • The preparation method of r, s-Gaoyichun
  • The preparation method of r, s-Gaoyichun
  • The preparation method of r, s-Gaoyichun

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Prepare Gao Yichun according to the following steps:

[0036] S1. Extraction: Take 13.3 kg of Radix Radix Radix as raw material, crush and sieve, dissolve in distilled water according to the ratio of material to liquid 1:6, ultrasonically extract for 60 minutes at a power of 60W, stir every 20 minutes, and let stand for 60 minutes after each ultrasonic extraction , Stir once every 30 minutes during this operation, extract 4 times in this way, filter, take the filtrate, and store it separately. The filter residue is extracted 3 times repeatedly according to the above operation, and the filtrates are combined. Use sodium hydroxide to adjust the pH of the water extract to 10, then use ethyl acetate to extract, extract 3 times, combine the ethyl acetate layers, and concentrate under low pressure to remove the ethyl acetate to obtain the extract mainly containing R, S-Caurus spring 27.21 gram.

[0037] S2. High-speed countercurrent chromatographic separation: configure a la...

Embodiment 2

[0045] Prepare Gao Yichun according to the following steps:

[0046] S1. extraction: same as step S1 in embodiment 1;

[0047] S2. High-speed countercurrent chromatographic separation: similar to step S2 in Example 1, the difference is that the volume ratio of ethyl acetate-n-butanol-ethanol-water is 7:1.5:0.5:8, and the retention value of the stationary phase is 81.3%;

[0048] S3. Separation by normal phase column chromatography: same as step S3 in Example 1 to obtain 9.48 g of R,S-Gaoyichun.

[0049] The purity of the obtained R,S-Gaoyichun by HPLC is 99.7%.

Embodiment 3

[0051] Prepare Gao Yichun according to the following steps:

[0052] S1. extraction: same as step S1 in embodiment 1;

[0053] S2. High-speed countercurrent chromatographic separation: similar to step S2 in Example 1, the difference is that the volume ratio of ethyl acetate-n-butanol-ethanol-water is 9:0.5:1.5:10, and the retention value of the stationary phase is 83.7%;

[0054] S3. Separation by normal phase column chromatography: same as step S3 in Example 1 to obtain 9.53 g of R,S-Gauyichun.

[0055] The purity of the obtained R,S-Gaoyichun by HPLC is 99.3%.

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Abstract

The invention discloses a method for preparing R,S-epigoitrin. The preparation method comprises the following steps: S1, extracting, namely by taking radix isatidis herbs as raw materials, performing ultrasonic extraction by distilled water, performing solvent extraction, and concentrating so as to obtain an extract containing R,S-epigoitrin mainly; S2, performing high-speed countercurrent chromatographic separation, namely performing high-speed countercurrent chromatographic elution separation on the extract, receiving the fraction, collecting the fraction containing a target product so as to obtain crude R,S-epigoitrin; and S3, performing normal phase column chromatography isolation, namely performing normal phase column chromatography isolation on the crude R,S-epigoitrin, thereby obtaining the target product. The R,S-epigoitrin prepared by the method disclosed by the invention is high in quality and large in single preparation, does not have any influence on the sample activity and does not cause any additional pollution. The product can be used for medicines, cosmetics, health care products and the like.

Description

technical field [0001] The invention relates to the technical field of extraction and separation of active ingredients of traditional Chinese medicines. Specifically, the invention relates to a preparation method of R,S-Gauyichun. Background technique [0002] R, S-Gaoyichun is an effective active ingredient in Radix isatidis, which has significant antiviral activity. The traditional method for preparing R, S-Gaoyichun basically adopts macroporous resin column separation, and mostly uses the method of macroporous resin column separation chromatography, normal phase column chromatography and reverse phase column chromatography, but adopts this The sample prepared by this method has low yield, small amount of preparation, and low purity, so it cannot be prepared on a large scale. In addition, this method also has the disadvantages of high pollution, long time consumption and high cost, and the original biological activity of the sample is greatly reduced due to the use of a l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D263/16
CPCC07D263/16
Inventor 黄启吟曾仑连林生
Owner UNO SCI CO LTD