Preparation method for standardized extracts of eucommia ulmoides pinoresinol diglucoside

A technology of pinoresinol diglucoside and extract, which is applied in the field of extracting active ingredients of plants, can solve problems such as unstable quality and efficacy, and difficulty in controlling the content of active ingredients, so as to achieve reduced usage, lower production costs, and high extraction efficiency Effect

Inactive Publication Date: 2014-05-28
JISHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As of 2013, there are 95 enterprises in China that have obtained registration and production approval documents for Eucommia traditional Chinese medicine preparations and health care products, mainly including Eucommia wine, Eucommia granules, Eucommia Jiangya Tablets, Eucommia Jiangya Capsules, Eucommia Pills, Eucommia Oral Liquid, etc. Dosage forms, manufacturers mostly use Eucommia decoction pieces as raw materials, the content of active ingredients in the product is difficult to control, and the quality and efficacy are unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 1000g of Eucommia bark, crush it, pass through a 20-mesh sieve, put it into a 20L ultrasonic-assisted extraction tank, add 15L of purified water, stir, heat it to 50°C, extract for 60min, and centrifugally filter; the centrifugate passes through a 0.1μm microporous filter, fine filtrate Ultrafiltration through a 50,000Da polysulfone roll-type membrane, the ultrafiltration retentate is reused as extraction process water, and the ultrafiltration dialysate is adsorbed on a macroporous resin; the adsorption column is 30×400mm, the resin model is D101, and the saturated adsorption capacity of PDG is 56.0mg / g. The volume on the column is 10.5BV (column volume, the same below), the flow rate is 2BV / h, until the point of PDG leakage occurs (the PDG content in the effluent is ≥0.1mg / ml, the same below), and the concentration is 30% and 50% Ethanol-water solution was used for gradient elution, the eluate was collected in sections, thin-layer spotting was detected, the same co...

Embodiment 2

[0024] Take 1000g of eucommia bark, crush it, pass through a 40-mesh sieve, put it into a 20L microwave-assisted extraction tank, add 12L of purified water, add an appropriate amount of sulfuric acid, and adjust the pH value to 4; add 84g of cellulase, heat to 50°C, and enzymatically hydrolyze for 2 hours. Centrifugal filtration; the centrifugate is passed through a 0.1μm microporous filter, the fine filtrate is passed through a 50,000Da polysulfone roll-type membrane ultrafiltration, the ultrafiltration retentate is reused as extraction process water, and the ultrafiltration dialysate is adsorbed on a macroporous resin; the adsorption column is 30×400mm , Resin model AB-8, PDG saturated adsorption capacity 62.29mg / g, loading volume 10.5BV, flow rate 2BV / h, until PDG leakage occurs; elute with 50% ethanol-water solution, collect the eluate in sections , thin-layer spotting detection, combining the same components; upper C 18 Reverse-phase silica gel column chromatography, flow...

Embodiment 3

[0026] Take 1000g of Eucommia bark, crush it, pass through a 60-mesh sieve, put it into a 20L microwave-assisted extraction tank, add 10L of purified water, heat it to 40°C, extract for 45 minutes, and centrifugally filter; 50000Da polysulfone roll-type membrane ultrafiltration, the ultrafiltration retentate is reused as extraction process water, and the ultrafiltration dialysate is adsorbed on a macroporous resin; the adsorption column is 30×400mm, the resin model is S-8, and the saturated adsorption capacity of PDG is 63.89mg / g , the amount on the column is 8.5BV, the flow rate is 2BV / h, until the point of PDG leakage; elute with 50% ethanol-water solution, collect the eluate in sections, detect by thin layer spotting, and combine the same components; above C 18 Reverse-phase silica gel column chromatography, flow rate 2BV / h, until the PDG breakthrough point is saturated and adsorbed; elute with 30% methanol-water solution, flow rate 0.5-1.0BV / h, collect eluate in sections, a...

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Abstract

The invention provides a preparation method for standardized extracts of eucommia ulmoides pinoresinol diglucoside. The method comprises the following steps: crushing dry eucommia ulmoides skin raw materials into 20-80 mesh, extracting for 1-2h according to material-liquid ratio of 1:(10-15), performing solid-liquid separation by using a centrifuge, performing micropore refined filtration, enabling the refined filtration liquid to pass through an ultrafiltration membrane to be separated, adsorbing by using macroporous adsorptive resin, eluting, concentrating the eluent, performing column chromatography by using C18 reverse phase silica gel for purification, performing secondary chromatography on the chromatography eluent by using polyamide columns and the like for purification, performing vacuum concentration on the secondary chromatography eluent, and then freeze-drying, so as to obtain eucommia ulmoides pinoresinol diglucoside standardized extracts at different purity levels. The preparing method is high in extracting efficiency and wide in technological applicability, can be used for producing standardized extracts at different purity levels according to different consumer market requirements of eucommia ulmoides health products, besides, facilitates the reduction of use amount of organic solvents, saves energy, reduces carbon emission, and reduces production cost and environmental pollution.

Description

technical field [0001] The invention relates to the extraction of effective plant components, in particular to a method and application of extracting pinoresinol diglucoside standard extract from eucommia bark as a raw material. Background technique [0002] Eucommia ulmoides is a precious and nourishing Chinese herbal medicine in my country. Eucommia ulmoides Oliv.) plant, used to use dry bark as medicine, has many functions such as nourishing liver and kidney, strengthening bones and muscles, lowering blood pressure, anti-abortion, etc., and "Shen Nong's Herbal Classic" is listed as the top grade. [0003] Modern pharmacological research shows that the secondary metabolites of Eucommia mainly include lignin, phenylpropanoids, iridoids, flavonoids, polysaccharides and other major components, as well as pinoresinol diglucoside, Eucommia gum, peach leaf, etc. Active ingredients such as coralline, β-sitosterol, chlorogenic acid, and betulin. Its medicinal functions and effec...

Claims

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Application Information

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IPC IPC(8): C07H15/26C07H1/08
CPCY02P20/10
Inventor 彭密军吕强彭胜王志宏王文茂
Owner JISHOU UNIVERSITY
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