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Extraction method and application of falcate dolichos root or leaf glucoside A and total saponins of falcate dolichos root or leaf

A technology of cannabis medicine and glycoside, which is applied in the field of preparation of cannabinoid glycoside A and total saponins of cannabis medicine, can solve problems such as adverse reactions, failure to prevent tissue damage, joint destruction and deformity, and achieve low price and significant anti-immunity Inflammatory action, definite curative effect

Active Publication Date: 2013-11-06
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although NSAIDs are often used as first-line drugs for the treatment of rheumatoid arthritis, they all have obvious adverse reactions. The relief of symptoms is mainly due to their anti-inflammatory effects, but cannot prevent tissue damage, joint destruction and deformity.
Although DMARDs that improve the condition can improve symptoms, these drugs have obvious adverse reactions, such as gastrointestinal mucosal damage leading to peptic ulcer, liver damage, rash, etc.

Method used

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  • Extraction method and application of falcate dolichos root or leaf glucoside A and total saponins of falcate dolichos root or leaf
  • Extraction method and application of falcate dolichos root or leaf glucoside A and total saponins of falcate dolichos root or leaf
  • Extraction method and application of falcate dolichos root or leaf glucoside A and total saponins of falcate dolichos root or leaf

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of cannabinoid total saponins and cannabinoid glycoside A

[0050] The preparation of the total saponins of the cannabis medicine: get 250g of the cannabis medicine medicinal material granules, place in a 5L round-bottomed flask, add 10 times the weight of the cannabis medicine medicinal material granules with a volume concentration of 60% ethanol, soak for 2 hours, and extract by reflux in a water bath. Extract three times, and the extraction time is 2, 1.5, and 1 hour respectively, and the filtrates are combined. The filtrate recovered ethanol under reduced pressure until it had no alcohol smell, and then dried it under reduced pressure at 60°C to dryness to obtain about 55 grams of total cannabinoid saponins (as determined by HPLC, the content of cannabinoid glycoside A was ≥52%).

[0051] The preparation method of cannabinoid glycoside A: take 250g of cannabis medicinal material granules, place them in a 5L round-bottomed flask, add 10 times the weight o...

Embodiment 2

[0053] The structure identification of cannabinoid glycoside A extracted in Example 1 was carried out.

[0054] Cannabinoid A, the compound has the formula C 37 h 58 o 11 , white powder, easily soluble in methanol, ethanol and water; melting point: m.p.295-297℃;

[0055] MS data (combined with figure 1 ): EI-MS (70eV) m / z, [M] - 677.4 (100); IR: 3400, 2930, 1695, 1445, 1260, 1165 cm -1 , indicating that there are phenolic hydroxyl groups, carbonyl groups and double bonds;

[0056] UV: Carry out full-band scanning under ultraviolet 190-400nm, and find that there is maximum absorption at 195nm;

[0057] H NMR spectroscopy (combined with figure 2 ): 1 H-NMR (DMSO-d6, 500MHz) δ: 5.5654 (1H, m, J=10.08Hz, H-12), 4.7265(1H, d, J=4.12, H-3), 4.5022(1H, m, J =9.95Hz, H-2), 2.0242(s, 2H, H-2), 1.6229 (1H, s, H-6), 1.0279, 0.8144, 0.9455;

[0058] NMR carbon spectrum: 13 C-NMR (DMSO-d6, 500MHz) data are shown in Table 1;

[0059] According to the above physical and chemic...

Embodiment 3

[0065] Content determination of cannabinoid glycoside A and total saponins of cannabinoids

[0066] 1. Chromatographic conditions

[0067] Agilent 1100 high performance liquid chromatography, the chromatographic column is Agilent TC-C18 (4.6×250 nm, 5 μm); detection wavelength: 203 nm; mobile phase: A is CH 3 CN, B is 0.1% phosphoric acid aqueous solution, gradient elution [0~8 min, 30%~40% A, 8~15 min, 40%~65% A, 15~20 min, 65%~75% A], Flow rate: 1.0 mL·min -1 , column temperature: 30°C, injection volume: 20 μL.

[0068] 2. Preparation of test solution

[0069] 2.1 Configuration of standard solution: Accurately weigh 2.4 mg of cannabinoid glycoside A standard dried to constant weight, add methanol to a 10 mL volumetric flask, and shake well to obtain 0.24 mg·mL -1 cannabinoid glycoside A standard.

[0070] 2.2 Preparation of cannabinoid glycoside A and cannabinoid total saponins sample solution:

[0071] Precisely weigh 12.8 mg of the total saponin sample of the cannabi...

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PUM

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Abstract

The invention discloses an extraction method of falcate dolichos root or leaf glucoside A. The method comprises the following steps: (1) taking falcate dolichos root or leaf herbs, adding alcohol aqueous solution for reflux extraction, wherein the weight of the alcohol aqueous solution is 6-12 times of that of falcate dolichos root or leaf herbs; (2) recovering the falcate dolichos root or leaf extract solution obtained from the step 1 under reduced pressure to alcohol till no alcohol taste exists, and adding water or alcohol to liquid medicine; (3) adding hydrochloric acid into the liquid medicine obtained from the step 2 till the pH value is 1-6, and adding sodium chloride into the liquid medicine till the salt concentration to 0.1-2mol / L; (4) placing the liquid medicine obtained from the step (3) on a macroporous adsorption resin column for separation; (5) cleaning and purifying with alcohol aqueous solution, of which the volume is 4-10 times of the column volume of the macroporous adsorption resin column, eluting with alcohol aqueous solution, of which the volume is 4-10 times of the column volume of the macroporous adsorption resin column, collecting the eluant, and drying to obtain falcate dolichos root or leaf glucoside A. The invention further discloses an extraction method of total saponins of falcate dolichos root or leaf, and the application of the falcate dolichos root or leaf glucoside A, the total saponins of falcate dolichos root or leaf, falcate dolichos root or leaf glucoside A hydrolysate and salt thereof and falcate dolichos root or leaf glucoside A derivate in preparing immune-inflammation resistant drugs.

Description

technical field [0001] The invention relates to a preparation method and application of cannabinoid glycoside A and total saponins of cannabinoids. Background technique [0002] Cannabis is the root or leaf of the leguminous plant Dolichos falcatus Kalcatus Klein, also known as Ma Li Ma, Ma San Duan, Dou Ye Bai Bu Huan Yang, etc. This product is pungent, numb and warm. It is distributed in Yunnan, Sichuan, Gansu and other places in my country, especially in Yunnan, which has abundant plant resources. It has the effects of expelling wind and activating blood circulation, stopping bleeding and relieving pain. In Yunnan, it is mainly used for fractures, bruises, rheumatism pain, external use to treat traumatic bleeding, and also has anti-cancer and diuretic effects. At present, the main chemical components of marijuana are triterpenoid saponins and alkaloid compounds. The extraction process of these compounds in the prior art is complicated, and the purity of the extract is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/256A61K36/48A61K31/704A61P19/02A61P19/06A61P29/00
Inventor 梅之南陈旅翼邓旭坤林亲雄兰洲周永强齐炼文
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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