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Novel method for efficiently extracting total alkaloids from wild thermopsis lanceolata in Greater Khingan Mountains

A technology of total alkaloids and biological enzymes, applied in the direction of organic chemistry, can solve the problems of low extraction purity and low extraction rate, and achieve the effect of increasing extraction speed, increasing active ingredient content, and high product purity

Active Publication Date: 2014-03-12
HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of conventional techniques such as low extraction rate and low extraction purity, and provide a method that mainly adopts biological enzymatic hydrolysis technology, ultrahigh pressure coupling subcritical water extraction, and adopts high-speed countercurrent chromatography (HSCCC) to separate and purify the total alkaloid method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: A method of adopting biological enzymatic hydrolysis technology, ultra-high pressure coupling subcritical water extraction, enzymatic separation and purification, and high-speed countercurrent chromatography separation and purification to finally obtain high-purity total alkaloids. The steps are as follows:

[0019] (1) Biological wall breaking: Add pectinase, cellulase, and hemicellulase (1:1:1) to 2kg of herbaceous bean seeds for enzymolysis, the enzyme concentration is 0.3g / kg, and the pH value is adjusted to 3 , enzymatic hydrolysis time 2h at 40°C;

[0020] (2) Ultra-high pressure extraction: add subcritical water, add according to the ratio of material to liquid of 1:8, pressurize with 200MPa pressure for 5min, pressurize twice;

[0021] (3) Separation and purification by enzymatic method: add papain and amylase (1:1) to the extract, the addition amount is 1‰, degrade the protein and starch in the extract into small molecules and remove them, and imp...

Embodiment 2

[0028] Embodiment 2: A method for obtaining high-purity total alkaloids by adopting biological enzymatic hydrolysis technology, ultra-high pressure coupling subcritical water extraction, enzymatic separation and purification, and high-speed countercurrent chromatography separation and purification, the steps are as follows:

[0029] (1) Biological wall breaking: Add pectinase, cellulase, and hemicellulase (1:2:1) to 5 kg of grazing bean seeds for enzymolysis, the enzyme concentration is 0.4 g / kg, and the pH value is adjusted to 4 , enzymatic hydrolysis time 3h at 45°C;

[0030] (2) High-pressure extraction: add subcritical water at a ratio of 1:10 to liquid, pressurize at 400MPa for 6 minutes, and pressurize twice;

[0031] (3) Separation and purification by enzymatic method: add papain and amylase (2:1) to the extract, the addition amount is 1.2‰, degrade the protein and starch in the extract into small molecules and remove them, and improve the difficulty of filtering the wa...

Embodiment 3

[0038] Embodiment 3: A method of adopting biological enzymatic hydrolysis technology, ultra-high pressure coupling subcritical water extraction, enzymatic separation and purification, and high-speed countercurrent chromatography separation and purification to finally obtain high-purity total alkaloids, the steps are as follows:

[0039] (1) Biological wall breaking: Add pectinase, cellulase, and hemicellulase (1:2:2) to 2kg of herbaceous bean seeds for enzymolysis, the enzyme concentration is 0.5g / kg, and the pH value is adjusted to 3 , enzymatic hydrolysis time 2h at 50°C;

[0040] (2) High-pressure extraction: add subcritical water according to the ratio of material to liquid of 1:12, pressurize at 300MPa for 4 minutes, and pressurize twice;

[0041] (3) Separation and purification by enzymatic method: add papain and amylase (1:2) to the extract, the addition amount is 1.5‰, degrade the protein and starch in the extract into small molecules and remove them, and improve the d...

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Abstract

The invention belongs to the field of natural organic chemistry and relates to a method for extracting and purifying total alkaloids from wild thermopsis lanceolata in Greater Khingan Mountains and particularly relates to a method for finally obtaining high-purity total alkaloids by using a biological enzymolysis technology and through ultrahigh pressure coupled subcritical water extraction, separation and refining by using an enzymatic method as well as separation and purification by using a high-speed counter-current chromatography. The method has the advantages that 1, the effective components of the alkaloids are rapidly dissolved out and the high activity is kept by using a biological exine detaching technology, and the method is carried out at normal temperature and is low in energy consumption and capable of realizing industrial production; 2, the subcritical water is nontoxic and pollution-free, so that the activity of an extract is not damaged; the operation cost is low, the extract is easy to be separated from a product, and large-scale industrial production can be realized; 3, the high-speed counter-current chromatography has the advantages of flexibility in operation, high efficiency, high separation speed, large preparation amount, low expense and the like, and can be used for industrial application. By using the method, the obtained total alkaloids are high in content and high in purity up to 95.8%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a new method for extracting total alkaloids from Daxing'anling wild horse beans, in particular to a method for extracting total alkaloids by means of ultra-high pressure coupled subcritical water extraction and high-speed countercurrent chromatography for separation and purification of total alkaloids new method. Background technique: [0002] Muma bean, also known as lanceolata Huanghua. Perennial herb, 10-40 cm high, glabrous throughout. Rhizome slender, light yellowish brown, with a few fibrous roots. Stems erect, slightly branched, with fine longitudinal striations on the surface. 3 compound leaves, alternate; leaflets obovate-oblong or oblanceolate, 2.5-8.5 cm long, 7-20 mm wide, apex acute, base cuneate, upper smooth, lower densely pubescent; Stipules 2, opposite, base united, raceme terminal; bracts 3, base united; flowers about 3 cm long; calyx tubular, about 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/18C07D471/22
CPCC07D471/18C07D471/22
Inventor 张亚红信小娟
Owner HEILONGJIANG DINGHENGSHENG PHARM CO LTD
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