Method for preparing salidroside

A technology of salidroside and Rhodiola grandiflora, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problem of small amount of preparation by high-performance liquid chromatography, which is not suitable for industrialized large-scale production, and rhodiola To solve the problems of low content of tianosin, to achieve the effect of simple purification and refining process, treatment of cardiovascular and cerebrovascular diseases, and improvement of resource utilization

Active Publication Date: 2011-02-16
KANGMEI PHARMA
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Problems solved by technology

The content of salidroside prepared by this method is low, and the cost is high, so it is not suitable for industrialized large-scale production
Ding Chaowu et al. ("Research on the preparation method of salidroside and salidroside aglycone standard", Journal of Analytical Testing, 1997, 16 (1): 38) separated and prepared by chemical and high-performance liquid phase preparative chromatography, and the obtained product High purity, but the amount of HPLC preparation is small and cannot be mass-produced
Ge Yongchao et al. ("Improvement of the preparation process of salidroside", Chinese Journal of Medicinal Chemistry, 1994, 4(3): 196) performed four kinds of column chromatography of polyamide, reversed-phase macroporous resin, silica gel and dextran gel. Combined use to prepare salidroside, this method has many kinds of separation media, and the cost is high, so it is not suitable for industrialized large-scale production

Method used

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  • Method for preparing salidroside
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  • Method for preparing salidroside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Study on Extraction Technology of Rhodiola daflora

[0038] In this example, the extraction method, extraction solvent, raw material particle size, soaking time, and extraction conditions in the extraction process of Rhodiola daflora were studied respectively.

[0039] 1. Investigation of extraction method

[0040] Take 3 parts of Rhodiola grandiflora medicinal materials that have been passed through a 50-mesh sieve, each 10 g, and extract with hot reflux respectively (add 10 times the amount of water each time, heat at 100 ° C, extract 3 times, and extract 3 hours each time); ultrasonic Extraction (add 10 times the amount of water each time, ultrasonic frequency 45KHz, extract 3 times, extract 1 hour each time); microwave extraction (add 10 times the amount of water each time, microwave power 462w, extract 3 times, extract 1.5 minutes each time ); the extract is filtered, concentrated under reduced pressure to a relative density of about 1.00 (measured at 2...

Embodiment 2

[0081] Example 2 Study on Purification Process of Rhodiola daflora

[0082] When the ethanol content in the extract reaches 60% to 70%, except for tannins and resins, other impurities have basically been precipitated and removed. If ethanol is added in two times, the concentration will gradually increase, and finally reach 75% to 85%. The effect of removing impurities is better, so choose two alcohol precipitation methods to remove impurities.

[0083] 1. Investigation of the first alcohol precipitation process

[0084] The relative density of the extract, alcohol precipitation concentration, and alcohol precipitation time are the main factors affecting the purification process. For these three factors, we choose L 9 (3 4 ) Orthogonal experiments are optimized, and three conventional levels are selected in each factor to consider, and Table 8A is a factor level table:

[0085] Table 8A Alcohol precipitation process factor level table

[0086]

[0087] Take 9 parts of ...

Embodiment 3

[0119] Example 3 Research on the Refining Technology of Rhodiola daflora

[0120] In this example, the resin type and purification process conditions in the refining process of Rhodiola daflora were studied respectively.

[0121] 1. Selection of macroporous resin model

[0122] Take NK-2 (purchased from Tianjin Fine Chemical Co., Ltd.), SP825 (purchased from Japan Mitsubishi Chemical Industry), D101 (purchased from Japan Mitsubishi Chemical Industry), D301 (purchased from Japan Mitsubishi Chemical Industry), AB-8 (purchased from Japan Mitsubishi Chemical Industry Co., Ltd.), AB-8 (purchased from Japan Mitsubishi Chemical Industry Co., Ltd. factory), HP-20 (purchased from Mitsubishi Chemical), SP700 (purchased from Mitsubishi Chemical), S-8 (purchased from Anhui Samsung Resin Technology Co., Ltd.) 8 different models have been pretreated (pretreatment process: with Soak the newly purchased resin in 0.5BV of ethanol for 24 hours, then alternately elute with 3 times the volume ...

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Abstract

The invention provides a method for preparing salidroside, which comprises the following steps: 1) extraction: adding water into a Rhodiola crenulata (Hook. f. et Thoms.) H. Ohba medicinal material, performing microwave extraction, filtering, concentrating and obtaining concentrate; 2) purification: performing secondary alcohol precipitation of the concentrate obtained by the step 1) and obtaining filtrate; and 3) refining: loading the filtrate obtained by the step 2) on a macroporous resin, eluting, concentrating, drying and obtaining the salidroside. The preparation method of the invention has the advantages of high extraction efficiency, simple process, capability for industrial production and the like.

Description

technical field [0001] The invention relates to a method for preparing salidroside. Background technique [0002] The medicinal material used in the present invention is Rhodiola grandiflora, derived from the main activity of the root or rhizome of Rhodiola crenulata (Latin name: Rhodiola crenulata (Hook.f.et Thoms.) H.Ohba) of Crassulaceae Rhodiola plant The ingredient is salidroside. Rhodia daflora is mainly produced in Tibet, northwestern Yunnan, and western Sichuan. It grows in grasslands and shrubs on hillsides at an altitude of 2,800 to 5,600 meters. It can grow in harsh and changeable natural environments. It is a highly adaptable species. plant. Traditional medicine believes that Rhodiola daflora can replenish qi and activate blood, dredge meridians and relieve asthma, and is used for qi deficiency and blood stasis, chest pain and heartache, stroke hemiplegia, fatigue and asthma. Rhodiola rosea mainly contains glycosides, flavonoids, polysaccharides, tannins, vola...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/08C07H15/18
Inventor 闵建华许冬瑾向飞军吴晓东陈华师
Owner KANGMEI PHARMA
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