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Method for preparing matrine from euchresta tubulosa dunn

A technology of matrine and bean root, applied in the field of natural product preparation, can solve the problem of not using nuclear magnetic resonance method and the like, and achieve the effects of saving resources, reducing production costs, and reducing environmental pollution emissions

Inactive Publication Date: 2020-06-23
长沙湘资生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are 14 alkaloids isolated from this genus of plants. Li Ruocun et al. isolated matrine, oxymatrine and cytisine from the root of Bean spp., but they were only analyzed and identified by chemical and infrared spectroscopy. The more precise nuclear magnetic resonance method (NMR) is not used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 100 kg of leaves of the root of the calyx tuberosa and crush them, add 300L of ethanol solution to carry out high-temperature extraction at 85°C for 3 hours, filter to obtain filtrate I and filter residue I; add 15L of Aspergillus niger liquid to ferment at room temperature for filter residue I, and then add 200L of ethanol solution for 85 ℃ for 3 hours at high temperature, and filtered to obtain filtrate II; filtrate I and filtrate II were combined, concentrated under reduced pressure at 60°C to 10L, extracted with 30L ethyl acetate to obtain an aqueous phase; the pH of the aqueous phase was adjusted to 8, and 20L of The butanol phase was extracted with alcohol to obtain the butanol phase; the butanol phase was concentrated to 1L under reduced pressure at 60°C, put on the ADS-7 column, and eluted with 70% ethanol aqueous solution to obtain 12L eluent I; Concentrate under reduced pressure at 60°C to 0.8L, crystallize overnight at 4-8°C, and filter to obtain 368g of ...

Embodiment 2

[0025] Take 200 kg of the leaves of the root of the tuber calyx and crush them, add 600L of ethanol solution to carry out high-temperature leaching at 85°C for 3 hours, filter to obtain filtrate I and filter residue I; add 30L of Aspergillus niger liquid to ferment for filter residue I at room temperature for 6 days, then add 400L of ethanol solution for 85 ℃ for 3 hours at high temperature, and filtered to obtain filtrate II; filtrate I and filtrate II were combined, concentrated under reduced pressure at 60°C to 20L, extracted with 60L ethyl acetate to obtain the water phase; the pH of the water phase was adjusted to 8, and 40L of The butanol phase was extracted with alcohol to obtain the butanol phase; the butanol phase was concentrated to 1L under reduced pressure at 60°C, put on the ADS-7 column, and eluted with 70% ethanol aqueous solution to obtain 20L eluent I; Concentrate under reduced pressure at 60°C to 1.5L, crystallize overnight at 4-8°C, and filter to obtain 735g ...

Embodiment 3

[0027] Take 400 kg of leaves of the root of the syringa tuberosa and crush them, add 1000L ethanol solution to extract at 85°C for 3 hours, filter to obtain filtrate I and filter residue I; add 50L Aspergillus niger liquid to ferment for filter residue I at room temperature for 6 days, then add 1000L ethanol solution for 85 ℃ and high temperature for 3 hours, and filtered to obtain filtrate II; filtrate I and filtrate II were combined, concentrated under reduced pressure at 60°C to 40L, extracted with 120L ethyl acetate to obtain the water phase; the pH of the water phase was adjusted to 7.5, and 180L of Extract the butanol phase with alcohol to obtain the butanol phase; concentrate the butanol phase to 4L under reduced pressure at 60°C, put it on the ADS-7 column, and elute with 70% ethanol aqueous solution to obtain 40L eluent I; eluate I Concentrate under reduced pressure to 2L at 60°C, crystallize overnight at 4-8°C, and filter to obtain 1.68g of matrine product. The conte...

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PUM

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Abstract

The invention provides a method for preparing matrine from euchresta tubulosa dunn. The method comprises the following steps of: taking and smashing the euchresta tubulosa dunn, adding an ethanol solution, carrying out high-temperature digestion at a temperature of 80-90 DEG C for 1-3 h, and filtering to obtain first filter liquor and first filter slags; adding 5-10% of aspergillus niger liquids into the first filter slags, carrying out room-temperature filtration at a room temperature for 3-8 days, then, adding the ethanol solution, carrying out the high-temperature digestion at a temperatureof 80-90 DEG C for 1-3 h, and filtering to obtain second filter liquor; combining the first filter liquor with the second filter liquor, carrying out vacuum concentration, and carrying out extractionby ethyl acetate of two times to four times of volume to obtain an aqueous phase; regulating the pH of the aqueous phase to 7.5-8, and carrying out extraction by butanol of two times to four times ofvolume to obtain a butanol phase; concentrating the butanol phase, placing an ADS-7 column, and carrying out elution by the ethanol solution of four time to six times of column volume to obtain firsteluent; and concentrating the first eluent, carrying out overnight crystallization at a temperature of 4-8 DEG C, and filtering to obtain a matrine product.

Description

[0001] Technical field [0002] The invention relates to a method for preparing matrine from the root of Bean calyx, belonging to the technical field of natural product preparation. Background technique [0003] Guan'e bean root is a plant of the genus Fabaceae, also known as E bean root, Hudoulian, bean root, and opium seven (Xiangxi area). Bean root plants contain alkaloids, flavonoids, steroids, volatile oil and other components. This genus contains a variety of flavonoids, 86 of which have been obtained from this genus, one of which is flavonoid glycosides, and the rest are flavonoid aglycones. Thirteen flavonoids, including 6 euchretins (A~E, I) and 7 euchretinones (euchretin a1, a4, a14, a15, b2) were isolated from the root of Euchretin euchretin. ,b16,b17). There are 14 alkaloids isolated from this genus of plants. Li Ruocun et al. isolated matrine, oxymatrine and cytisine from the root of Bean spp., but they were only analyzed and identified by chemical and infrared...

Claims

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Application Information

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IPC IPC(8): C12P17/18
CPCC12P17/182
Inventor 董爱文姚姝凤成江
Owner 长沙湘资生物科技有限公司
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