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A method for preparing salidroside chemical reference substance from Rhodiola angustifolia root

A technology of salidroside chemistry and Rhodiola angustifolia, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve problems such as cumbersome process, unsuitable for industrial production, time-consuming alcohol precipitation process loss, etc. , to achieve the effect of simple process, good decolorization effect and low price

Inactive Publication Date: 2018-08-24
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, Chinese patent (CN101974045A) reports that salidroside with a purity of about 92% can be obtained from Rhodiola daflora by steps such as microwave extraction, secondary alcohol precipitation and macroporous resin purification. The loss in the sinking process is relatively large, which is not suitable for industrial production, but there is no report on the preparation of salidroside from the root of Rhodiola angustifolia

Method used

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  • A method for preparing salidroside chemical reference substance from Rhodiola angustifolia root
  • A method for preparing salidroside chemical reference substance from Rhodiola angustifolia root

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Effect test

Embodiment 1

[0027] Embodiment 1 A kind of method for preparing salidroside chemical reference substance from rhodiola angustifolia root, comprises the following steps:

[0028] ⑴ Silica gel column chromatography enrichment:

[0029] 3.0 Kg Rhodiola root ethanol extract was separated by silica gel column chromatography, eluted with 5 times the column volume of chloroform-methanol-water mixed solvent, and the fractions were collected in 200 mL each, and detected by thin-layer chromatography, wherein the developing agent was chloroform -Methanol-water mixed solvent, the color developer is concentrated sulfuric acid ethanol solution with a volume concentration of 10%, and the fraction with an Rf value of 0.5~0.7 is combined; Under the condition of decompression drying, 1050.8 g of crude salidroside was obtained in the form of brown yellow powder.

[0030] Among them: the ethanol extract of Rhodiola angustifolia root refers to crushing the roots of Rhodiola angustifolia to 50 mesh, adding eth...

Embodiment 2

[0039] Embodiment 2 A kind of method for preparing salidroside chemical reference substance from rhodiola angustifolia root, comprises the following steps:

[0040] ⑴ Silica gel column chromatography enrichment:

[0041] 1.0 Kg Rhodiola angustifolia root ethanol extract was separated by silica gel column chromatography, eluted with 10 times column volume of chloroform-methanol-water mixed solvent, and fractions were collected in 500 mL portions, and detected by thin-layer chromatography, wherein the developing solvent was Chloroform-methanol-water mixed solvent, the developer is concentrated sulfuric acid ethanol solution with a volume concentration of 10%, and the fractions with an Rf value of 0.5~0.7 are combined; Under the condition of ℃, it was dried under reduced pressure to obtain 348.3 g of crude salidroside in the form of brown yellow powder.

[0042] Among them: Rhodiola angustifolia root ethanol extract refers to crushing the root of Rhodiola angustifolia to 100 mes...

Embodiment 3

[0051] Embodiment 3 A kind of method for preparing salidroside chemical reference substance from root of rhodiola angustifolia comprises the following steps:

[0052] ⑴ Silica gel column chromatography enrichment:

[0053] 0.3 Kg Rhodiola angustifolia root ethanol extract was separated by silica gel column chromatography, eluted with 15 times column volume of chloroform-methanol-water mixed solvent, and fractions were collected in 300 mL portions, and detected by thin-layer chromatography, wherein the developer was Chloroform-methanol-water mixed solvent, the developer is concentrated sulfuric acid ethanol solution with a volume concentration of 10%, and the fractions with an Rf value of 0.5~0.7 are combined; 110.6 g of crude salidroside in the form of brown yellow powder was obtained by drying under reduced pressure at ℃.

[0054] Among them: Rhodiola angustifolia root ethanol extract refers to crushing the roots of Rhodiola angustifolia to 60 mesh, adding methanol according...

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Abstract

The invention relates to a method for preparing a salidroside chemical reference substance from Rhodiola kirilowii root, which comprises the following steps: (1) silica gel column chromatography enrichment: carrying out silica gel column chromatography separation and elution on a Rhodiola kirilowii root alcohol extract, carrying out thin-layer chromatography detection, and drying under reduced pressure to obtain a brown yellow powdered salidroside crude product; (2) microporous resin impurity removal: dissolving the salidroside crude product, separating through a microporous resin column, eluting, and drying under reduced pressure to obtain a salidroside component; and (3) reversed liquid-phase preparative chromatography refinement: dissolving the salidroside component, filtering through a microporous filter membrane, separating through a high-performance reversed liquid-phase preparative chromatography column, collecting the target chromatogram peak fraction in the preparative chromatogram, and drying the target chromatogram peak fraction under reduced pressure to obtain the white powdered salidroside reference substance. The method is simple in technique and can easily implement scale-up production.

Description

technical field [0001] The invention relates to a preparation method of a chemical reference substance, in particular to a method for preparing a salidroside chemical reference substance from roots of Rhodiola angustifolia. Background technique [0002] Rhodiola angustifolia ( Rhodiola kirilowii (Regel) Maxim.) Department of Crassulaceae ( Crassulaceae ) Rhodiola ( Rhodiola L. )plant. "Tibetan Medicine" records: Rhodiola angustifolia root is used as medicine, which can be used to clear away heat and reduce fever, detoxify, prevent plague, treat pneumonia, diarrhea, and swelling of limbs. Modern pharmacological studies have found that Rhodiola angustifolia has the functions of preventing altitude sickness, promoting blood circulation and removing blood stasis, improving hypoxia tolerance, radiation protection, and improving cardiovascular system function. Rhodiola angustifolia is widely distributed in Qinghai Province and has a large amount of resources, but it has not...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/18C07H1/08
Inventor 党军张莉梅丽娟邵赟王启兰陶燕铎赵建强
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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