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Extracting method of hernandezine

A technology of hylandrazine and its extraction method, which is applied in the field of extraction and separation of traditional Chinese medicines, can solve problems such as the undiscovered industrial extraction and purification method of hylandrazine, and achieve the effects of reducing the dissolution of impurities, short extraction time and good separation effect

Inactive Publication Date: 2013-01-16
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] After searching the literature, no relevant reports on the industrial extraction and purification method of Helandizine have been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Grind the dried root of the golden silk horsetail, take 2kg, add 1.0% hydrochloric acid aqueous solution to soak for 4 hours, ultrasonic treatment for 40 minutes, filter the obtained extract on HZD-2 cation exchange resin, first wash it with deionized water until it is neutral, and then wash it with 8LpH10 85% ethanol solution for elution, the eluent was concentrated under reduced pressure, the pH was adjusted to 10.5, extracted with chloroform, the chloroform layer was taken, and the chloroform was recovered to dry to obtain the crude product; Mix at 7:2:10, let it stand, separate the upper and lower phases, the lower phase is the stationary phase, and the upper phase is the mobile phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 850rpm, take the crude product dissolved in the upper phase and inject it into the chromatograph to control the flow The phase flow rate was 2ml / min, and the hylandrazine fraction was collected, concentrated, and ...

Embodiment 2

[0025] Grind the dried root of the golden horsetail, take 2kg, add 0.5% hydrochloric acid aqueous solution to soak for 3 hours, ultrasonically treat for 45 minutes, filter the obtained extract on D-151 cation exchange resin, wash it with deionized water until neutral, and then use 8LpH9 75% ethanol solution was eluted, the eluate was concentrated under reduced pressure, adjusted to pH 11.0, extracted with chloroform, the chloroform layer was taken, and the chloroform was recovered to dry to obtain the crude product; Mix for 6:1:8, let it stand, separate the upper and lower phases, the lower phase is the stationary phase, and the upper phase is the mobile phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 850rpm, take the dissolved crude product of the upper phase and inject it into the chromatograph, and control the flow The phase flow rate was 2ml / min, and the hylandrazine fraction was collected, concentrated, and dried to obtain coarse crystals; d...

Embodiment 3

[0027] Crush the dried root of the golden horsetail, take 5kg, add 1.2% sulfuric acid aqueous solution to soak for 5h, ultrasonic treatment for 60min, filter the obtained extract on HD-8 cation exchange resin, wash it with deionized water until it is neutral, and then wash it with 20LpH11 90% ethanol solution for elution, the eluent was concentrated under reduced pressure, the pH was adjusted to 10.0, extracted with chloroform, the chloroform layer was taken, the chloroform was recovered and dried to obtain the crude product; Mix at 6:2:10, let it stand, separate the upper and lower phases, the lower phase is the stationary phase, the upper phase is the mobile phase, turn on the high-speed countercurrent chromatograph, adjust the speed to 850rpm, take the crude product dissolved in the upper phase and inject it into the chromatograph to control the flow The phase flow rate was 2ml / min, and the hylandrazine fraction was collected, concentrated, and dried to obtain coarse crystal...

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Abstract

The invention discloses an extracting method of hernandezine. The extracting method comprises the steps as follows: crushing thalictrum glandulosissimum raw material; adding 0.4 to 1.2% of hydrochloric acid or sulfuric acid aqueous solution to extract; extracting up-liquid cation exchange resin column; washing to reach neuter with deionized water; eluting with alkaline solution; concentrating the eluant in a pressure reduced way; adjusting pH (Potential of Hydrogen) to reach 10 to 11; extracting with chloroform; concentrating the extracting liquid; then separating according to high-speed counter-current chromatography and preparative liquid chromatography; collecting target component; and drying at low temperature so as to obtain the hernandezine product. The extracting method disclosed by the invention is low in energy consumption, brings less pollution, and has high product content that is up to over 98%, therefore, the possibility on industrial automatic production is given.

Description

Technical field [0001] The present invention belongs to the field of Chinese medicine extraction and separation technology, and specially involves a method of extract of Hilanzine. Background technique [0002] Hernandezine (Hernandezine), also known as golden ponytail alkali, molecular formula is C 39 H 44 N 2 O 7 , Molecular weight is 652.79, which is a kind of albumin alkaloid, MP.120-122 ° C.Mainly existing in the genus plants of the Moso family, such as the winged Tang pine grass, the golden silk ponytail, and the Persian Tang pine grass. [0003] Golden Horsailian THALICTRUM GLANDULOSISIMUM (Fin.et gagn.) W.t.wang et S.H.H.Wang, alias, polyphono, is distributed in the Dali generation of Dali, Yunnan, my country, and Hailanzine is mainly separated from the golden ponytail. [0004] Pharmacological studies have shown that Hailanzinezine has external collagen, ADP, and A 23187 It has a significant inhibitory effect with the aggregation of AA -induced plate plate plates. Becaus...

Claims

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Application Information

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IPC IPC(8): C07D491/18
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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