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Method for preparing glycine betaine chemical reference substances from boxthorn leaves

A technology of Lycium barbarum leaves and betaine, which is applied in chemical instruments and methods, organic chemistry, cyanide reaction preparation, etc., can solve the problems of large loss in the crystallization process, cumbersome process, and no literature reports on the preparation of betaine. The effect of low cost, simple process and easy batch preparation

Active Publication Date: 2015-08-12
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

[0003] At present, there are few reports on the preparation of betaine from plants. Chinese patent (101863784B) reported that anhydrous betaine with a purity of about 98% was obtained by using 8 to 10 steps of the synthesis method. The process is cumbersome and the loss in the crystallization process is relatively large.
There is no literature report on the preparation of large-scale acquisition of betaine from plants

Method used

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  • Method for preparing glycine betaine chemical reference substances from boxthorn leaves
  • Method for preparing glycine betaine chemical reference substances from boxthorn leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0025] ⑴Water extraction:

[0026] 1.0 Kg of Lycium barbarum leaves were dried in the shade and crushed, then added analytically pure water 4 times its mass, extracted once at 60°C for 2 hours each time, filtered and combined the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.

[0027] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.06 MPa and a temperature of 70 °C.

[0028] ⑵ Silica gel column enrichment:

[0029] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 20 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 1000 mL each, and detected by thin-layer chromatography, wherein the developi...

Embodiment 2

[0039] Example 2 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0040] ⑴Water extraction:

[0041] 10.0 Kg of Lycium barbarum leaves were dried in the shade and crushed, then added analytical pure water 10 times its mass, extracted 3 times at 90°C for 1 hour each time, filtered and combined the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.

[0042] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.09 MPa and a temperature of 50 °C.

[0043] ⑵ Silica gel column enrichment:

[0044] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 8 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 2000 mL each, and detected by thin-layer chromatography, wherein the develop...

Embodiment 3

[0054] Example 3 A method for preparing betaine chemical reference substances from leaves of Lycium barbarum, comprising the following steps:

[0055] ⑴Water extraction:

[0056] 5.0 Kg Lycium barbarum leaves were dried in the shade, crushed, added analytical pure water 7 times its mass, extracted twice at 75°C for 3 hours each time, filtered and combined with the filtrate A, and the filtrate A was dried under reduced pressure to a paste, that is, Brown-black solid wolfberry leaf water extract.

[0057] Wherein: the conditions of decompression drying refer to a vacuum degree of 0.08 MPa and a temperature of 60 °C.

[0058] ⑵ Silica gel column enrichment:

[0059] After the water extract of Lycium barbarum leaves was separated by silica gel column chromatography, it was eluted with 10 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected at 1000 mL each, and detected by thin-layer chromatography, wherein the developing solv...

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Abstract

The invention relates to a method for preparing glycine betaine chemical reference substances from boxthorn leaves. The method includes the following steps: (1), drying the boxthorn leaves in the shade, smashing the boxthorn leaves, adding analysis pure water to perform extraction, and filtering and drying the mixture under reduced pressure into paste to obtain brown black solid boxthorn leaf water extracts; (2), performing elution after subjecting the boxthorn leaf water extracts to silica gel column chromatography separation, collecting cut fractions according to 1000-2000mL / part, and combining the cut fractions with Rf values being 0.1-0.2 through thin-layer chromatography detection; drying the cut fractions with the Rf values being 0.1-0.2 under reduced pressure to obtain brown powdery glycine betaine crude products; (3), dissolving the glycine betaine crude products in ethanol solutions, performing filtering and hydrophilic liquid phase preparative chromatography separation to collect main chromatographic peak cut fractions in preparative chromatograms, and drying the chromatographic peak cut fractions under reduced pressure to obtain the white powdery reference substances with purity larger than 99%. The method has the advantages of simple technology and proneness to mass production.

Description

technical field [0001] The invention relates to a method for preparing a betaine chemical reference substance, in particular to a method for preparing a betaine chemical reference substance 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 buds of the wolfberry plant in Ningxia are commonly known as Tianjingcao. It is recorded in "Compendium of Materia Medica": Tianjingcao can "eliminate annoyance and improve intelligence, replenish five labors and seven injuries, strengthen the heart, remove wind between the skin and bones, eliminate heat and poison, loose sores". Betaine is a quaternary amine alkaloid with high content in wolfberry leaves. Modern pharmacological studies have shown that betaine has the functions of enhancing immunity, lowering blood fat, anti-oxidation, anti-tumor, promoting fat m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/12C07C227/40
Inventor 梅丽娟党军张莉王启兰陶燕铎邵赟刘增根江磊
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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