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Extraction and purification method of saikosaponin

A technology of saikosaponin and extraction liquid, which is applied in the directions of pharmaceutical formulations, medical preparations containing active ingredients, plant raw materials, etc., can solve the problem of low saikosaponin, and achieves improved biological activity, wide technical application, and medicinal saponins. small loss effect

Active Publication Date: 2011-08-31
SICHUAN DE PEI YUAN TRADITIONAL CHINESE MEDICINE SCI & TECH DEV CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Regarding the separation and purification of saikosaponin, although macroporous resins have been widely used in the prior art to separate and purify saikosaponin, most of them are directly loaded after dilution of the extract. The content of saikosaponin in the separated material is particularly high. low content of d

Method used

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  • Extraction and purification method of saikosaponin
  • Extraction and purification method of saikosaponin
  • Extraction and purification method of saikosaponin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] 1. Determine the content of saikosaponin a and d in the sample by HPLC

[0065] The high performance liquid chromatography conditions are as follows:

[0066] Chromatographic column: Diamonsil C18 (250×4.6mm);

[0067] Mobile phase: acetonitrile-methanol-water gradient elution, the elution program is shown in Table 1:

[0068] Table 1. Elution program

[0069] time (minutes)

Acetonitrile (volume%)

Water (volume%)

0-50

25-90

75

50-55

90

10

[0070] Flow rate: 1ml / min;

[0071] Column temperature: 30°C;

[0072] Detection wavelength: 210nm;

[0073] Injection volume: 10 microliters.

[0074] 2. The colorimetric method for the determination of total saponins is as follows:

[0075] Take saikosaponin a as a standard, draw a certain amount of sample, add 0.1% ethanol solution of p-dimethylaminobenzaldehyde, first react in a water bath at 70°C for 10 minutes, let it cool to room temperature, add 4ml of phosphoric acid, an...

Embodiment 2

[0079] The content detection method of saikosaponin a+d and total saikosaponin in this embodiment is the same as that in embodiment 1.

[0080] Example 3

[0081] Take 1 kg of Bupleurum bupleurum medicinal residues with supercritical extraction of volatile oil, add 60% (v / v) of 10 times the volume of medicinal materials, and soak in ethanol with a pH value of 8 for 24 hours, then percolate at a flow rate of 6 mL / min, collect The percolation solution is concentrated under reduced pressure at 70°C to form a dilute extract, and the concentrated extract is diluted with alkaline water with a pH value of 8 to a content of 0.05g / mL of total saplein Put the drug solution on a D101 macroporous resin column with a resin column diameter-to-height ratio of 1:2, let it stand for 3 hours for adsorption, stir for 5 hours, and then dynamically adsorb at a flow rate of 3BV / h, then wash the column with 6BV of water to remove impurities, and then use 4BV30 % (v / v) ethanol to remove impurities; ...

Embodiment 3

[0083] Example 4

[0084] Take 1 kg of fresh Bupleurum bupleuri, wash, slice, air / dry, crush to 10 mesh, add 70% (v / v) of 8 times the volume of the medicinal material, soak in ethanol with a pH value of 10 for 36 hours, and perform percolation. The percolation flow rate is 5mL / min, the percolation liquid is collected, concentrated under reduced pressure at 50°C to form a dilute extract, and then diluted with alkaline water with a pH value of 9 to dilute the concentrated extract until the total saponin content of Bupleurum is 0.03g / mL (based on crude drug The amount is recorded as 3g), put the diluted medicinal solution on the D101 macroporous resin column, the ratio of diameter to height of the resin column is 1:5, let it stand for adsorption for 4 hours, stir and adsorb for 7 hours, and then dynamically adsorb, the adsorption flow rate is 1BV / h, and then use 4BV Wash the column with water to remove impurities, and then use 4BV of 30% (v / v) ethanol to remove impurities;

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Abstract

The invention discloses an extraction and purification method of saikosaponin. The saponin part mainly contains saikosaponin a and saikosaponin d. The extract can be prepared by using a percolation method or a high-pressure percolation method, an ethanol solution is used for extracting bupleurum medicinal material, macroporous resin is used for purifying in the purification process, the total weight of the saikosaponin a and saikosaponin d in the prepared saikosaponin extract accounts for 30-60% of the weight of the extract, and the weight of the total saponins accounts for 50-80% of the weight of the extract. The method disclosed by the invention is simple to operate, has the advantages of low production cost, energy saving and high extraction efficiency, and is suitable for industrialized production.

Description

technical field [0001] The invention discloses a method for extracting and purifying effective components of traditional Chinese medicines, in particular to a method for extracting and purifying saikosaponin, and belongs to the technical field of extracting and separating effective components of medicines. Background technique [0002] Bupleurum is a common medicinal material, and the 2010 edition of "Chinese Pharmacopoeia" stipulates that Bupleurum is a Umbelliferae plant Bupleurum chinense DC. or Bupleurum angustifolia B. scorzonerifolium Dried root of Willd. Bupleurum has the effects of soothing the liver and relieving depression, relieving the exterior and harmonizing the interior. The active components of Bupleurum bupleuri are mainly volatile components and saponins. The types of saponins are complex, mainly including saikosaponins a, c, d, b1, b2, h, etc., among which saikosaponins a and d have the ability to inhibit thrombosis , increase glucocorticoid and other...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/233
Inventor 余伯阳马璇戚进寇俊萍马家骅索志荣杨兴旺杨占国
Owner SICHUAN DE PEI YUAN TRADITIONAL CHINESE MEDICINE SCI & TECH DEV CO LTD
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