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Method for preparing rutin and quercetin chemical reference substances simultaneously from lycium barbarum leaves

A technology of quercetin chemistry and reference substances, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve the problems of large loss in the crystallization process, cumbersome process, no literature reports, etc., and achieve easy operation , simple process and low price

Active Publication Date: 2015-09-09
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent (102718820B) reports that rutin with a purity of 96% can be obtained from rutin-rich raw materials such as Sophora japonica, buckwheat, and asparagus by using 6-8 steps such as organic solvent extraction, alkali dissolution, acid precipitation, and crystallization. The process is cumbersome. And the crystallization process loses a lot
However, there is no literature report on the simultaneous purification and preparation of rutin and quercetin

Method used

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  • Method for preparing rutin and quercetin chemical reference substances simultaneously from lycium barbarum leaves
  • Method for preparing rutin and quercetin chemical reference substances simultaneously from lycium barbarum leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 A method for simultaneously preparing rutin and quercetin chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0027] ⑴Microporous resin impurity removal:

[0028] 200 g of the Lycium barbarum leaf ethanol extract prepared by the conventional method is dissolved with 60% methanol solution with a volume fraction of 5 times of its mass, and is filtered to obtain filtrate A, which is separated by a microporous resin column on the filtrate A and then washed with water of 2 times the column volume. , 20% methanol solution, and 70% methanol solution to carry out step gradient elution, collect 70% methanol water eluate, and dry the methanol water eluate under reduced pressure to obtain 32.4 g of crude rutin and quercetin.

[0029] Among them: the ratio of ethanol extract of wolfberry leaf to microporous resin was 1 g: 30 mL.

[0030] The conditions for drying under reduced pressure refer to a vacuum degree of 0.06 MP...

Embodiment 2

[0041] Example 2 A method for simultaneously preparing rutin and quercetin chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0042] ⑴Microporous resin impurity removal:

[0043] 500 g of Lycium barbarum leaf ethanol extract prepared by the conventional method is dissolved with 30% methanol solution with volume fraction of 10 times of its mass, and is filtered to obtain filtrate A, which is separated by microporous resin column on the filtrate A with water successively with 5 times of column volume , 35% methanol solution, and 70% methanol solution for step gradient elution, collected 70% methanol water eluate, and dried the methanol water eluate under reduced pressure to obtain 80.4 g of crude rutin and quercetin.

[0044] Among them: the ratio of ethanol extract of wolfberry leaf to microporous resin was 1 g: 30 mL.

[0045] The conditions for drying under reduced pressure are 0.09 MPa and 50°C.

[0046] The microporous r...

Embodiment 3

[0056] Example 3 A method for simultaneously preparing rutin and quercetin chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0057] ⑴Microporous resin impurity removal:

[0058] 1000 g of Lycium barbarum leaf ethanol extract prepared by the conventional method is dissolved with 50% methanol solution with volume fraction of 8 times of its mass, and is filtered to obtain filtrate A, which is separated by microporous resin column on the filtrate A with water of 3 times of column volume successively. , 30% methanol solution, and 70% methanol solution for step gradient elution, collected 70% methanol water eluate, and dried the methanol water eluate under reduced pressure to obtain 159.6 g of crude rutin and quercetin.

[0059] Among them: the ratio of ethanol extract of wolfberry leaf to microporous resin was 1 g: 30 mL.

[0060] The conditions of drying under reduced pressure are 0.07 MPa and 60°C.

[0061] The microporous re...

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Abstract

The invention relates to a method for preparing rutin and quercetin chemical reference substances simultaneously from lycium barbarum leaves. The method comprises the following steps: (1) carrying out impurity removal with microporous resin: dissolving a lycium barbarum leaf alcohol extract with a methanol solution, filtrating the solution, loading the filtrate to a microporous resin column for separation, then, carrying out stepped gradient elution sequentially with water, a 20-35% methanol solution and a 70% methanol solution, collecting 70% methanol water eluate, and enabling the methanol water eluate to be subjected to reduced-pressure drying, thereby obtaining rutin and quercetin crude products; (2) enabling the rutin and quercetin crude products to be subjected to silicagel-column chromatographic separation, eluting, and combining fractions with the Rf value of 0.3-0.5; enabling the fractions to be subjected to reduced-pressure drying, thereby obtaining brown-yellow powdered rutin and quercetin components; and (3) refining with reversed phase liquid preparative chromatography: dissolving the rutin and quercetin components with a methanol solution, filtrating the solution, separating the filtrate with an efficient reversed phase liquid preparative chromatographic column, collecting two major chromatographic peak fractions from a preparative chromatogram, and enabling the chromatographic peak fractions to be subjected to reduced-pressure drying, thereby obtaining yellow powdered rutin and quercetin reference substances. The method is simple in process and facilitates large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a chemical reference substance, in particular to a method for simultaneously preparing rutin and quercetin chemical reference substances from wolfberry leaves. Background technique [0002] Lycium barbarum leaves belong to Solanaceae ( Solanaceae ) Lycium barbarum ( Lycium ) plant Ningxia Lycium barbarum ( Lycium barbarum L.) leaves. The tender stems, leaves or shoots of Ningxia wolfberry are commonly known as Tianjingcao. It is recorded in "Compendium of Materia Medica": Tianjingcao can "eliminate annoyance and improve intelligence, nourish five labors and seven injuries, strengthen heart energy, remove wind between skin and joints, eliminate heat and poison, loose sores". Modern studies have shown that wolfberry leaves are rich in flavonoids, which have various pharmacological activities such as lowering blood pressure, lowering blood lipids, and preventing cardiovascular diseases. ) components...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08C07D311/30C07D311/40
CPCC07D311/30C07D311/40C07H1/08C07H17/07
Inventor 梅丽娟党军张莉王启兰邵赟陶燕铎刘增根江磊
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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