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Method for extracting oxysophocarpine from Sophora davidii

A technology of oxidative sophocarpine and wolf tooth thorn flower, applied in the direction of organic chemistry and the like, can solve the problems of low collection rate, high flower collection rate, harmfulness, etc., and achieve the effects of simple operation process, wide source of raw materials and high product purity

Inactive Publication Date: 2017-06-13
刘煜华
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the total alkaloids of matrine prepared in this process, the extraction rate of sophocarpine and oxysophocarpine is extremely low, and the use of toluene in this process is harmful to human body, so it is difficult to popularize and apply
[0005] At present, only alkaloid extraction and series product development and utilization are carried out on the seeds of Spike thorn, but the seed setting rate of Spike thorn is extremely low, less than 10% of the flowers can mature into seeds, and more than 90% of the flowers will fall during the growth process Waste; in addition, the collection of spike seeds is difficult and the collection rate is low, while the flower collection rate is high and easy to collect

Method used

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  • Method for extracting oxysophocarpine from Sophora davidii

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Experimental program
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Effect test

Embodiment 1

[0024] Determination of the content of oxysophocarpine in the raw material Langya thorn flower

[0025] (1) Preparation of standard solution: Accurately weigh 10.0 mg of oxysophocarpine standard substance, dissolve it in ultrapure water and dilute it into a 10 mL volumetric flask to prepare a standard substance containing 1.00 mg / mL oxysophocarpine Mother liquor;

[0026] (2) Preparation of the sample solution: Accurately weigh 0.5 g of the Spike thorn flower sample, place it in a 100 mL Erlenmeyer flask, add 10 mL of analytically pure concentrated ammonia to make it wet, then add 30 mL of analytically pure chloroform, and shake for 30 min. After standing still for 4 hours, filter, extract the filter residue continuously for 3 times, combine the extracts, and then recover chloroform at 80°C to obtain a dry product, which is dilute to 25 mL with ultrapure water, filtered through a 0.5 μm microporous membrane, and collected The filtrate is the sample solution, for subsequent us...

Embodiment 2

[0030] A method for extracting oxysophocarpine from Spiny japonica, comprising the following steps:

[0031] (1) Pretreatment: weigh shiitake mushrooms, add water according to the ratio of material to liquid 1g: 30 mL, heat at 50°C for 40 minutes, filter after cooling, recycle shiitake mushrooms, and use the obtained shiitake mushroom filtrate for use; The shiitake mushroom filtrate was mixed according to the material-to-liquid ratio of 1:8, soaked at 3°C ​​for 2 hours, stirred once every 20 minutes, and filtered to obtain pretreated wolf tooth thorns;

[0032] (2) Extraction: add 400mL of methanol solution to the wolf tooth thorn flower pretreated in step (1) according to the ratio of solid to liquid 1g: 8 mL, soak for 72 hours, collect the filtrate and filter residue after filtration, and filter the residue according to the ratio of solid to liquid 1g: 8 mL was soaked in 400mL methanol solution for 48 h, and the filtrate and filter residue were collected after filtration, an...

Embodiment 3

[0041] A method for extracting oxysophocarpine from Spiny japonica, comprising the following steps:

[0042] (1) Pretreatment: weigh shiitake mushrooms, add water according to the material-liquid ratio of 1g: 30 mL, heat at 40°C for 60 minutes, filter after cooling, recycle shiitake mushrooms, and use the obtained shiitake mushroom filtrate for later use; mix 50g of wolf tooth thorn flowers with the above-mentioned The shiitake mushroom filtrate was mixed according to the ratio of material to liquid 1:8, soaked at 6°C for 2 hours, stirred once every 20 minutes, and filtered to obtain pretreated wolf tooth thorns;

[0043] (2) Extraction: add 400mL of methanol solution to the wolf tooth thorn flower pretreated in step (1) according to the ratio of solid to liquid 1g: 8 mL, soak for 72 hours, collect the filtrate and filter residue after filtration, and filter the residue according to the ratio of solid to liquid 1g: 8 mL was soaked in 400mL methanol solution for 48 h, and the f...

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Abstract

The invention discloses a method for extracting oxysophocarpine from Sophora davidii. The method includes the steps of firstly, mixing mushrooms with water, heating, filtering, and using filtrate to preprocessing the Sophora davidii; secondly, using a solution containing at least one organic solvent to soak and extract the preprocess Sophora davidii twice, combining two filtrate, performing vacuum concentration on the filtrate to obtain crude oxysophocarpine extract, using an acetic acid solution to soak and extract filter residues twice, combining two filtrate, and performing vacuum extraction on the filtrate to obtain crude oxysophocarpine extract; combining the obtained crude oxysophocarpine extract, performing water precipitation on the combined crude oxysophocarpine extract to remove impurities, collecting filtrate, performing vacuum concentration, vacuum drying, silica gel column separation, crystallization separation and recrystallization on the filtrate, and drying to obtain the oxysophocarpine. The method has the advantages that the Sophora davidii can be recycled, the method is simple to operate, high in extraction rate and high in product purity, the oxysophocarpine can be obtained by direct extraction, and the purity of the oxysophocarpine can reach above 99%.

Description

technical field [0001] The invention belongs to the technical field of biological extraction, and in particular relates to a method for extracting oxysophocarpine from wolf tooth thorn flowers. Background technique [0002] Spike thorn, also known as white thorn flower, is a perennial shrub of the genus Sophora genus Fabaceae. It mostly grows in sunny slopes or valleys at an altitude of 400-1500m. It is widely distributed in North China, Jiangsu, Zhejiang, Hubei, Henan, Shaanxi, Gansu and Southwest China. Wait for the province. The roots, stems, leaves, flowers, fruits and seeds of wolf tooth thorn contain alkaloids, including oxymatrine, sophocarpine, sophoridine and other alkaloids. Wolf tooth thorn is widely used as a folk medicinal material. Sophocarpine oxide is the main active ingredient of Chinese herbal medicine. , antiasthma, antiarrhythmia, etc., is an important raw material for the development of various human medicines, cleaning products and insecticidal biopes...

Claims

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Application Information

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IPC IPC(8): C07D471/22
CPCC07D471/22
Inventor 刘煜华周宝龙王光中牛森
Owner 刘煜华
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