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Preparation method for pure anhydroicaritin

A technology to remove icariin and epimedium, which is applied in the direction of organic chemistry, can solve the problems of cost increase, and achieve the effects of saving production cost, improving purity, and simple operation process

Inactive Publication Date: 2013-06-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of these methods are completed based on icariin as a substrate [document 1. Beijing Shenaoji Pharmaceutical Technology Co., Ltd. CN 101302548A, the preparation method of 2007 icariin; document 2. Yi Peng, Yu Pei et al. Chinese Medicinal Materials. 33(11), 1804-1806, 2010, a new method for preparing icariin], which increases the cost

Method used

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  • Preparation method for pure anhydroicaritin
  • Preparation method for pure anhydroicaritin
  • Preparation method for pure anhydroicaritin

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Take 200 mg of Shaanxi Epimedium medicinal material, add 4 ml of ethanol with a volume concentration of 70%, conduct ultrasonic extraction for 30 minutes, obtain the ethanol extract of Epimedium by suction filtration, and repeat the ultrasonic extraction twice. Merge the ethanol extract of Epimedium and set the volume to 9ml ( figure 1 ). Add 3 ml of HCL with a mass concentration of 37%, and hydrolyze at 100° C. for 7 hours. Methanol was removed from the hydrolyzate using a rotary evaporator. The product was dissolved in water, centrifuged at 2000 r / min for 5 minutes, the supernatant was discarded, and the procedure was repeated three times. PH test paper is used to detect the supernatant, so that the pH is not less than 6.5, and the precipitate is filtered to obtain the crude icariin. The crude product of anhydroicariin was dissolved in 5ml methanol ( figure 2 ), through 0.45um micro-membrane filtration, the samples filtered out by the micro-membrane were loaded a...

Embodiment 2

[0034] Take 500 mg of Epimedium medicinal material from Northeast China, add 5 ml of ethanol with a volume concentration of 90%, conduct ultrasonic extraction for 10 minutes, obtain alcoholic extract of Epimedium by suction filtration, and repeat ultrasonic extraction twice. The alcoholic extracts of Epimedium were combined and the volume was adjusted to 16ml. Add 8 ml of HCL with a mass concentration of 37%, and hydrolyze at 95° C. for 8 hours. Methanol was removed from the hydrolyzate by rotary evaporation. The product was dissolved in water, centrifuged at 2000 r / min for 5 minutes, the supernatant was discarded, and the procedure was repeated three times. PH test paper is used to detect the supernatant, so that the pH is not less than 6.5, and the precipitate is filtered to obtain the crude icariin. The crude dehydroicariin was dissolved in 10ml of methanol, filtered through a 0.45um micromembrane, and the sample filtered through the micromembrane was loaded for analysis,...

Embodiment 3

[0036] Take 1.5 g of Epimedium medicinal material produced in Guangxi, add 15 ml of ethanol with a volume concentration of 40%, conduct ultrasonic extraction for 50 minutes, obtain an alcoholic extract of Epimedium by suction filtration, and repeat ultrasonic extraction twice. The alcoholic extracts of Epimedium were combined and the volume was adjusted to 42ml. Add 30 ml of HCL with a mass concentration of 37%, and hydrolyze at 90° C. for 9 hours. Methanol was removed from the hydrolyzate by rotary evaporation. The product was dissolved in water, centrifuged at 2000 r / min for 5 minutes, the supernatant was discarded, and the procedure was repeated three times. PH test paper is used to detect the supernatant, so that the pH is not less than 6.5, and the precipitate is filtered to obtain the crude icariin. The crude dehydrated icariin was dissolved in 20ml of methanol, filtered through a 0.45um micromembrane, and the sample filtered through the micromembrane was loaded for an...

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Abstract

The invention relates to a preparation method for pure anhydroicaritin. Medical materials of herba epimedii of different producing areas serve as raw materials, and through extraction of herba epimedii flavonoid, hydrolyzation of hydrochloric acid and purification of the reversion phase efficient preparation chromatography, the pure anhydroicaritin with purity larger than 95% is obtained. The preparation method for the pure anhydroicaritin is simple in processing steps, high in purity, low in cost and capable of large-scale production.

Description

[0001] Technical Field The present invention relates to a method for preparing pure epimeditin anhydrous. It mainly includes the extraction of epimedium flavonoids, hydrochloric acid hydrolysis and efficient preparation and purification of hydrolyzed products. The structure of anhydroicariin is as follows: [0002] Background technique [0003] Epimedii (Herba Epimedii) belongs to the Berberidaceae (Berberidaceae) Epimedium genus, is commonly used in traditional Chinese medicine. Existing pharmacological experiments show that Epimedium has antiviral effects, improves immunity, and treats osteoporosis. Epimedium flavonoids are a class of compounds with the largest content in Epimedium. These compounds are formed by adding different sugar groups at the 3 and 7 sites with anhydroicariin as the core Different kinds of compounds. More and more experiments have shown that the flavonoids in Epimedium can be converted into anhydroicariin in the intestine, so it reflects that anh...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
Inventor 肖红斌杨乾栩卓荣杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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