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Preparation, quality control method and application of composition of active ingredients of bitter herb

A quality control method and active ingredient technology, which can be applied to medical preparations containing active ingredients, drug combinations, plant/algae/fungus/moss components, etc. It can solve problems that affect the separation effect, are difficult to separate out, and have a large production load.

Active Publication Date: 2012-02-29
沈阳双鼎制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of Kudiezizi extract is disclosed, which adopts the method of repeatedly adjusting the acidity and alkalinity of alcohol solution. Since luteolin-7-O-β-D-glucuronide is unstable in alkaline solution, it is prone to oxidation and Ring-opening reaction, and the cichoric acid in Kudiezi is not easy to precipitate in acidic solution, resulting in low yield and loss of a large amount of active ingredients
At the same time, although the patent provides that the content of the extract luteolin 7-O-β-D-glucuronide is only about 8%, this content has neither reached the standard of the second-class raw material drug for intravenous injection, that is, 80% above
[0008] 4. The invention patent of application number 200410078168.0 "a preparation containing the extract of Aphrodisiac clamosa and its preparation method" discloses a composition containing total flavonoids Not less than 80, of which the flavonoid luteolin 7-O-glucuronic acid is not less than 24, and the adenosine is not less than 0.18. Column chromatography, on the one hand, the flocculation process is complicated to operate, the product yield is low, and non-drug impurities are easily brought in; on the other hand, simple water or alcohol-treated extracts are subjected to column chromatography, and the impurity content is large, which affects the separation effect , resulting in heavy production load and low finished product content
Furthermore, this method is not conducive to the extraction of cichoric acid

Method used

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  • Preparation, quality control method and application of composition of active ingredients of bitter herb
  • Preparation, quality control method and application of composition of active ingredients of bitter herb
  • Preparation, quality control method and application of composition of active ingredients of bitter herb

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 500g of Kudiezi medicinal material, dry it in an oven at 65-70°C, crush it to 40 mesh for later use, add 1 times the amount of water (mass), put it in a microwave oven for 5 minutes, and add a certain amount of microwave-treated material A certain amount of compound enzyme to fully enzymatically hydrolyze the material, then dry and pulverize the enzymatic hydrolyzate and put it into CO extraction 2 Take the kettle and carry out supercritical CO 2 Extraction: 95% ethanol and greater than 99.99% liquid CO 2 Mix according to 20:80, reach supercritical state through heat exchanger, and then pass into extraction kettle, extraction pressure is 32MPa, extraction temperature is 60°C, extraction time is 2h. Concentrate the extract, absorb the concentrate through an AB-8 resin column, wash it with 30% ethanol until it is colorless, and take the alcohol washing solution for concentration. Filter, adjust the pH value of the filtrate to 4-5, let stand, precipitate, and filter...

Embodiment 2

[0033] Take 500g of Kudiezi medicinal material, dry it in an oven at 65-70°C, crush it to 40 mesh for later use, add 1 times the amount of water (mass), put it in a microwave oven for 5 minutes, and add a certain amount of microwave-treated material A certain amount of compound enzyme to fully enzymatically hydrolyze the material, then dry and pulverize the enzymatic hydrolyzate and put it into CO extraction 2 Take the kettle and carry out supercritical CO 2 Extraction: 95% ethanol and greater than 99.99% liquid CO 2Mix according to 20:80, reach supercritical state through heat exchanger, and then pass into extraction kettle, extraction pressure is 32MPa, extraction temperature is 60°C, extraction time is 2h. Concentrate the extract, absorb the concentrate through an AB-8 resin column, wash it with 30% ethanol until it is colorless, and take the alcohol washing solution for concentration. Filter, adjust the pH value of the filtrate to 4-5, let stand, precipitate, and filter....

experiment example 1

[0087] Experimental Example 1 Dog Myocardial Ischemia Test

[0088] 1 Experimental materials

[0089] 1.1 Drugs and reagents

[0090] The active ingredient composition of Kudiezi can be obtained by the above-mentioned preparation method, and its properties are light yellow and white powder, odorless. Prepare the required concentration with 0.9% sodium chloride injection before use.

[0091] 1.2 Animals

[0092] Twenty-five dogs were used in the experiment, provided by the Experimental Animal Center of Shenyang Pharmaceutical University, weighing 7.5-10.0kg, and used both male and female.

[0093] 1.3 Instruments

[0094] SLY-808 intelligent eight-channel physiological recorder, Shanghai Keke Medical Model Co., Ltd.

[0095] Model 752 UV-Vis Spectrophotometer, Shanghai Analytical Instrument Factory

[0096] 2 Experimental methods

[0097] Effects on Myocardial Infarction Caused by Coronary Ligation in Anesthetized Dogs

[0098] Take 30 test dogs, both for ♀♂ and 7.5-10k...

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Abstract

The invention discloses a preparation method, a quality control method and an application of composition of active ingredients ob bitter herb. The composition of the active ingredients of the bitter herb disclosed by the invention mainly comprises cichoric acid and luteolin-7-O-beta-D-glucuronide, and content of the cichoric acid and the luteolin-7-O-beta-D-glucuronide is not less than 80%. An extraction method of the composition comprises that pretreatment is carried out by adopting an enzymatic method, then a supercritical fluid extraction method is adopted, and the obtained extract is respectively subjected to separating, purifying, concentrating and drying by virtue of an AB-8 resin column and a polyamide resin column so as to obtain the composition. Besides, the invention also relates to an application of the composition in preparation of modern bitter herb injection and treatment on coronary heart disease, angor pectoris, myocardial infarction and cerebral infarction and an application of the composition in content determination of the composition of the active ingredients of the bitter herb and quality control of bitter herb medicinal material.

Description

technical field [0001] The invention provides a Kudiezi active ingredient composition, and also relates to a preparation method of the composition and an application of the composition, which belong to the technical field of traditional Chinese medicine. Background technique [0002] Ixeris sonchifolia (Bge) Hance, commonly known as Kudiezi, Gypsophila, etc., is the biennial dry aboveground part of Ixeris sonchifolia (Bge) Hance in the family Asteraceae. It is mainly produced in Northeast my country, North China, etc. land. "Ministry of Health Drug Standards Inner Mongolia Sub-volume" records that the bitter, pungent, cool in nature, has appetizing, detoxifying, bone-setting, and removing swelling effects. Folks are mainly used to treat appendicitis, tonsillitis, and unknown swelling and pain. The research on Kudiezi medicinal materials and preparations has made great progress in recent years. According to literature reports, Kudiezi contains flavonoids, adenosine, lactone ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/28G01N30/02A61P9/10
Inventor 马占芝胡爽
Owner 沈阳双鼎制药有限公司
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