Preparation and purification method of lotus plumule total alkali perchlorate

A technology of total alkaloid and perchlorate of lotus root, applied in the direction of organic chemistry, etc., can solve the problems of difficult crystallization, difficult removal of reactants and by-products, and difficult recovery.

Pending Publication Date: 2022-04-15
FUJIAN UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] But, above method is all not suitable for the preparation and the purification of Lianxin total alkaloid perchlorate
Because the total alkaloids of Lianxin react with perchloric acid to form a salt, it is very easy to dissolve in the reaction solution and it is difficult to crystallize. Even if it is placed in a refrigerator at 4°C for several days, there is still no crystallization; The acid has a boiling point as high as 203°C and is difficult to recover, and the remaining reactants and by-products are difficult to remove

Method used

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  • Preparation and purification method of lotus plumule total alkali perchlorate
  • Preparation and purification method of lotus plumule total alkali perchlorate
  • Preparation and purification method of lotus plumule total alkali perchlorate

Examples

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Embodiment 1

[0038] A method for preparing and purifying perchlorate of total alkaloids of lotus heart, which is characterized in that, taking 1 part of total alkaloids of lotus heart powder, adding an appropriate amount of commercially available perchloric acid to completely dissolve it, and then adding an appropriate amount of purified water to dilute to perchloric acid With a mass concentration of 10%, add 1.5 times the volume of water-saturated dichloromethane to extract twice, combine the dichloromethane, recover, concentrate, and dry to obtain total alkaloid perchlorate 1 of lotus root.

Embodiment 2

[0040] A method for preparing and purifying perchlorate of total alkaloids of lotus heart, which is characterized in that, taking 1 part of total alkaloids of lotus heart powder, adding an appropriate amount of commercially available perchloric acid to completely dissolve it, and then adding an appropriate amount of purified water to dilute to perchloric acid The mass concentration is 1%, add 3 times the volume of water-saturated dichloromethane to extract once, combine the dichloromethane, recover, concentrate, and dry to obtain the total alkaloid perchlorate 2 of Lianxin.

Embodiment 3

[0042]A method for preparing and purifying perchlorate of total alkaloids of lotus heart, which is characterized in that, taking 1 part of total alkaloids of lotus heart powder, adding an appropriate amount of commercially available perchloric acid to completely dissolve it, and then adding an appropriate amount of purified water to dilute to perchloric acid The mass concentration is 40%, adding 0.25 times the volume of water-saturated dichloromethane to extract three times, combining the dichloromethane, recovering, concentrating, and drying to obtain the total alkaloid perchlorate 3 of Lianxin.

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Abstract

The invention relates to a method for preparing lotus plumule total alkali perchlorate from lotus plumule total alkali and purifying the lotus plumule total alkali perchlorate. The method comprises the following specific operation steps: taking 1 part of liensinine powder, adding a proper amount of commercially available perchloric acid to completely dissolve the liensinine powder, adding a proper amount of purified water to dilute the liensinine powder until the mass concentration of the perchloric acid is 1-40%, adding a proper amount of water-saturated dichloromethane to extract for 1-3 times, combining the dichloromethane, recovering, concentrating and drying to obtain the liensinine total alkali perchlorate. An existing alkaloid salt forming process usually adopts a method of firstly forming salt and then crystallizing in an organic solvent, but the crystallization time is long and the yield is low. Compared with the prior art, the method for preparing and purifying the lotus plumule total alkali perchlorate, provided by the invention, is simpler and more efficient, and is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the preparation technology of traditional Chinese medicine alkaloids, in particular to a method for preparing and purifying perchlorate of lotus root total alkaloids (hereinafter referred to as lotus root total alkaloids). Background technique [0002] The lotus seed heart is the dry young leaves and radicles of the mature seeds of the water lily family plant lotus (Nelumbo nucifera Gaertn). It is a variety recorded in the "Chinese Pharmacopoeia" in previous editions. The effect of heat, solid essence and hemostasis. Traditional Chinese medicine is used for the treatment of heat entering the pericardium, disharmony between heart and kidney, insomnia and nocturnal emission, blood heat and vomiting blood. [0003] Lieninin total alkaloids are the main active ingredients in lotus seeds, including liensinine, isoliensinine and methyl-liensinine, etc., which have a wide range of biological activities such as lowering blood pressure...

Claims

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Application Information

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IPC IPC(8): C07D217/20
Inventor 曾建伟褚剑锋谭春江林珊陈达鑫郑春松吴广文曹治云
Owner FUJIAN UNIV OF TRADITIONAL CHINESE MEDICINE
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