CN101817828B - Preparation of bergenin in aruneus dioicus - Google Patents

Abstract

The invention belongs to the technical field of the research and development of medical products, relating to preparation of bergenin in aruneus dioicus. A preparation method comprises the steps of: pulverizing dried aruneus dioicus, soaking for 10-12 hours in 50 percent of alcohol, carrying out ultrasound for 1-1.5 hours with the temperature of 30 DEG C and the power of 80W, repeating 3 times, filtering by using gauze, merging filtrate, concentrating, blending and suspending by using water, sequentially extracting by using petroleum ether, ethyl acetate and n-butyl alcohol, concentrating the recovered extracting solvent to obtain four parts, dissolving an ethyl acetate part by using methanol, blending a sample by using silicagel, loading on a silicagel column, assembling the column by using chloroform, carrying out gradient elution by using chloroform-methanol, merging similar fractions, concentrating, further carrying out chromatography by using the silicagel column, merging similar fractions, concentrating, separating out crystal and obtaining a bergenin monomer by using a recrystallization method. The bergenin has the main effect of relieving a cough and eliminating phlegm, also has the effects of anti-inflammation, liver protection, anti-ulcer, immune improvement and the like and can be further used for the research and development of corresponding preparation products used for clinical applications.

Description

The preparation of Bergeninum in the false dioicus

Technical field

Pharmaceutical prod research and development technical field under the present invention.The present invention relates to the preparation of Bergeninum in the false dioicus.It is cough-relieving apophlegmatic that product of the present invention mainly acts on, and also has anti-inflammatory, protects liver, effect such as antiulcer agent, raising immunity.Can further research and develop the corresponding preparations product is used for clinical.

Background technology

The present invention relates to false dioicus is the feedstock production Bergeninum.False rattletop Aruncus sylvester Kostel.ex Maxim. is the dry root of the false rattletop of the Rosaceae (Rosaceae) Goatsbeard (Aruncus).Another name: kerria grass fiber crops, medicinal function: expelling wind to resolve the exterior, activate blood and relax tendons.The area distributes: produce Heilungkiang, Jilin, Liaoning, Henan, Gansu, Shaanxi, Hunan, Jiangxi, Anhui, Zhejiang, Sichuan, Yunnan, Guangxi, Tibet.Be distributed in ground such as Soviet Union siberian, Japan, Korea abroad.

Bergeninum claims vakerin, bergenin, bergenit again, is the effective constituent of saxifragaceae plant Rhizome or herb of Purple Bergenia, Herba astilbes chinensis.Rhizome or herb of Purple Bergenia have antitussive action, is used for chronic bronchitis, has made tablet at present and has been used for clinical.Be characterized in that untoward reaction is little to the selective restraining effect of coughing centre, and use does not produce resistance continuously, but drug effect is not high, only be 1/7～1/4 of codeine phosphate, and internal metabolism is fast, bioavailability is not high.It is cough-relieving apophlegmatic that Bergeninum mainly acts on, but recent pharmacological evaluation is found effects such as Bergeninum also has anti-inflammatory, protects liver, antiulcer agent, raising immunity.

At present, for the domestic and international rarely seen report of the research of false rattletop plant chemical ingredient, can research and develop further that Bergeninum corresponding preparations product is used for clinical in the false rattletop.

Summary of the invention

1. one kind is the method for feedstock production Bergeninum with false dioicus, it is characterized in that comprising following process:

Step (one): get false rattletop dry root and pulverize, ultrasonic again 1h-1.5h behind the 50% alcohol immersion 10h-12h, temperature is 30 ℃, power is 80W, repeats 3 times, uses filtered through gauze then, obtains filtrate;

Step (two): the filtrate in the step () is merged, concentrate, concentrated solution water suspendible is used sherwood oil, ethyl acetate, n-butanol extraction successively, concentrates the recovery extraction solvent and obtains four positions;

Step (three): with the ethyl acetate extract dissolve with methanol in the step (two), with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform-methanol gradient elution;

Step (four): the similar flow point in the step (three) is merged, concentrate, get concentrated solution, with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform-methanol gradient elution;

Step (five): the similar flow point in the step (four) is merged, concentrate, get concentrated solution, separate out crystal;

Step (six): the crystal in the step (five) is obtained the Bergeninum monomer with ethyl alcohol recrystallization.

According to the present invention, " % " among the present invention is weight percent.

Embodiment

Of the present invention relating to false dioicus is that the feedstock production Bergeninum comprises following examples, and the following examples can further specify the present invention, but do not limit the present invention in any way.

Embodiment 1:

Step (one): get false rattletop dry root 2.3kg and pulverize, ultrasonic again 1h behind the 50% alcohol immersion 10h, temperature is 30 ℃, power is 80W, repeats 3 times, uses filtered through gauze then, obtains filtrate;

Step (two): the filtrate in the step () is merged, concentrate, concentrated solution water suspendible is used sherwood oil, ethyl acetate, n-butanol extraction successively, concentrates the recovery extraction solvent and obtains four positions;

Step (three): with the ethyl acetate extract 13.8g dissolve with methanol in the step (two), with going up 360g behind the 16g silica gel mixed sample, 100-200 order silicagel column is with chloroform dress post, chloroform-methanol gradient elution;

Step (four): the similar flow point in the step (three) is merged, concentrate, get concentrated solution, with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform one methyl alcohol gradient elution;

Step (five): the similar flow point in the step (four) is merged, concentrate, get concentrated solution, separate out crystal;

Step (six): the crystal in the step (five) is obtained Bergeninum monomer 4.8g with ethyl alcohol recrystallization.

Embodiment 2:

Step (one): get false rattletop dry root 2.5kg and pulverize, ultrasonic again 1.5h behind the 50% alcohol immersion 12h, temperature is 30 ℃, power is 80W, repeats 3 times, uses filtered through gauze then, obtains filtrate;

Step (two): the filtrate in the step () is merged, concentrate, concentrated solution water suspendible is used sherwood oil, ethyl acetate, n-butanol extraction successively, concentrates the recovery extraction solvent and obtains four positions;

Step (three): with the ethyl acetate extract 14g dissolve with methanol in the step (two), with going up 360g behind the 16g silica gel mixed sample, 100-200 order silicagel column is with chloroform dress post, chloroform-methanol gradient elution;

Step (four): the similar flow point in the step (three) is merged, concentrate, get concentrated solution, with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform-methanol gradient elution;

Step (five): the similar flow point in the step (four) is merged, concentrate, get concentrated solution, separate out crystal;

Step (six): the crystal in the step (five) is obtained Bergeninum monomer 5.0g with ethyl alcohol recrystallization.

The Bergeninum structure is identified

Compounds X: colourless prism-shaped crystallization (MeOH), 132～134 ℃ of mp.Dissolve in methyl alcohol, different hydroxyl oxime iron reacting positive, iron trichloride/Tripotassium iron hexacyanide reaction shows blue.UVλmax(nm)：275，220。EI-MSm/z：328·08(M-H)，328·08(M-H，11％)，312·07(M-H-CH3，70％)，234·06(M-H-CH3-C2H6O3，90％)，192·04(M-H-CH3-CH8O4，100％)。IRumaxcm-1：3?389·96，3?251·68(-OH)，2?951·87(-CH3)，2?892·28(-CH2-)，1?704·38(C＝O)，1612·27，1?528·64，1?464·03(aromatic)，1?343·83，1234·90(aromatic?C-O)，861·20(C-H)。1H-NMR(400MHz，C5D5N)δ：3·99(s，3H，-OCH3)，4·17～4·33(m，3H)，4·5(dd，J＝8·6，9·0Hz，1H)，4·65(，tJ＝9·78，1H)，4·72(d，J＝10·56Hz，1H)，5·27(d，J＝10·57Hz，1H)，7·6(s，1H，aromatic-H)；13C-NMR(400MHz，C5D5H)δ：119·528(C-1)，116·579(C-2)，149·402(C-3)，141·894(C-4)，152·769(C-5)，111·073(C-6)，165·454(C-7)，73·876(C-1′)，75·522(C-2′)，81·297(C-3′)，72·089(C-4′)，83·501(C-5′)，62·575(C-6′)，60·283(MeO)。Authenticating compound X is a Bergeninum.

Bergeninum

Claims (1)

1. one kind is the method for feedstock production Bergeninum with false dioicus, it is characterized in that comprising following process:

Step (one): get false rattletop dry root and pulverize, ultrasonic again 1h-1.5h behind the 50% alcohol immersion 10h-12h, temperature is 30 ℃, power is 80W, repeats 3 times, uses filtered through gauze then, obtains filtrate;

Step (two): the filtrate in the step () is merged, concentrate, concentrated solution water suspendible is used sherwood oil, ethyl acetate, n-butanol extraction successively, concentrates the recovery extraction solvent and obtains four positions;

Step (three): with the ethyl acetate extract in the step (two), use dissolve with methanol, with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform-methanol gradient elution;

Step (four): the similar flow point in the step (three) is merged, concentrate, get concentrated solution, with going up silicagel column behind the silica gel mixed sample, with chloroform dress post, chloroform-methanol gradient elution;

Step (five): the similar flow point in the step (four) is merged, concentrate, get concentrated solution, separate out crystal;

Step (six): the crystal in the step (five) is obtained the Bergeninum monomer with ethyl alcohol recrystallization.