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Method for preparing notoginsenoside R1 and ginsenoside Rg1, Re, Rb1 and Rd

A technology of notoginseng saponins and ginsenosides, which is applied in the fields of steroids and organic chemistry, which can solve the problems of prolonged analysis time and unfavorable separation and preparation of saponins, and achieve the effects of simple process, low cost and shortened production cycle

Inactive Publication Date: 2011-11-09
UNIVERSITY OF MACAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although in the analysis of ginsenosides, reversed-phase high-performance liquid chromatography is generally also used, but in order to separate ginsenosides Rg1 and Re, it is necessary to use a low proportion of acetonitrile, which greatly prolongs the entire analysis time, which is not conducive to the separation and preparation of saponins[ See, Wan JB, Lai CM, Li SP et al., J. Pharm Biomed Anal. 2006, 41, 274-279]

Method used

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  • Method for preparing notoginsenoside R1 and ginsenoside Rg1, Re, Rb1 and Rd
  • Method for preparing notoginsenoside R1 and ginsenoside Rg1, Re, Rb1 and Rd
  • Method for preparing notoginsenoside R1 and ginsenoside Rg1, Re, Rb1 and Rd

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Experimental program
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Effect test

Embodiment 1

[0035] 200g of notoginseng medicinal material powder, ultrasonically extracted with 1000ml of 70% ethanol for 2h, repeated three times to combine the extract, and evaporated the solvent in vacuo to obtain the extract. The above extract was fully dissolved in 200ml of 40% (v / v) ethanol-water. Apply the solution of the above extract to preparative reversed-phase high performance liquid chromatography, with Alltima C18 (250 × 22mm, 10 μ m) as a chromatographic column, 203nm detection, flow rate 6.0ml / min, 40% (v / v) ethanol-water System (Phase A) and 60% (v / v) ethanol-water system (Phase B) were used as the mobile phase for gradient elution, and the elution procedure was shown in Table 2. Notoginsenoside R1, ginsenoside Re, and Rg1 were collected respectively. , Rb1 and Rd elution peaks.

[0036] Table 2 Gradient elution program

[0037] time (min)

[0038] The collected liquids of ginsenosides were combined, the solvent was evaporated under reduced pressure, and vacuu...

Embodiment 2

[0040] Take 20 g of commercially available Panax notoginseng saponins, fully dissolve in 200 ml of pure water, apply the solution of the above extract to preparative reversed-phase high-performance liquid chromatography, use Alltima C18 (250 × 22 mm, 10 μm) as the stationary phase, 203 nm Detection, flow rate 6.0ml / min, 40% (v / v) ethanol-water system (A phase) and 60% (v / v) ethanol-water system (B phase) as mobile phase for gradient elution, elution program As shown in Table 2, the elution peaks of notoginsenoside R1, ginsenoside Re, Rg1, Rb1 and Rd were collected respectively (see Figure 5 ).

[0041] The collected liquids of ginsenosides were combined, the solvent was evaporated under reduced pressure, and vacuum freeze-dried to obtain freeze-dried powders of notoginsenoside R1, ginsenoside Rg1, Re, Rb1 and Rd monomer compounds.

Embodiment 3

[0043] 200g of notoginseng medicinal material powder, ultrasonically extracted with 1000ml of 70% ethanol for 2h, repeated three times to combine the extract, and evaporated the solvent in vacuo to obtain the extract. The above-mentioned extract is fully dissolved in 200ml water, applied to 500g D-101 macroporous adsorption resin, first eluted with 3000ml of pure water, then eluted with 30% (v / v) ethanol-water 6000ml, and finally washed with 3000ml 80% (v / v) ethanol-water is carried out eluting and combining respectively 30% and 80% ethanol-water eluate, evaporates solvent under reduced pressure, vacuum freeze-drying, obtain intermediate notoginseng protopanaxatriol type saponin and Protopanaxadiol saponins.

[0044] The protopanaxatriol-type saponins obtained by the above separation were applied to preparative reversed-phase high-performance liquid chromatography, with Alltima C18 (250 × 22mm, 10 μm) as the stationary phase, and 40% (v / v) ethanol-water system as the mobile ph...

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Abstract

The invention provides a method for simply, conveniently and quickly preparing notoginsenoside R1 and ginsenoside Rg1, Re, Rb1 and / or Rd, which can meet the requirement of industrial production and isenvironment-friendly. In the method, notoginseng extract and arasaponin or notoginsenoside intermediates are used as original materials, a preparative scale reversed phase high-performance liquid chromatography is adopted, and an ethanol-water system is used as a flow phase to carry out isocratic elution or gradient elution, wherein the ethanol-water system is an ethanol-water solution of 30 percent to 80 percent (V / V). The method has the advantages of simple process, no pollution, low cost and high purity, wherein the purity of products produced by the method is more than 97 percent.

Description

technical field [0001] The invention relates to a preparation method of active ingredients of traditional Chinese medicine, in particular to a preparation method of saponins in Panax notoginseng. Background technique [0002] Panax notoginseng is the dry root of Panax notoginseng (Burk.) F.H.Chen, a plant of Araliaceae. It is a famous and precious Chinese medicine in my country, and its main active ingredients are saponins. According to statistics, more than 50 kinds of dammarane-type triterpene saponins have been isolated from Panax notoginseng so far, among which notoginseng saponin R1, ginsenosides Rg1, Re, Rb1 and Rd are the main components. Panax notoginseng saponins have a wide range of pharmacological activities on the blood system, nervous system, cardiovascular system, immune system and metabolism [see, "Pharmacology and Application of Traditional Chinese Medicine (Second Edition)", edited by Wang Yusheng, Deng Wenlong, Xue Chunsheng, Pages 598-606, People's Health...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J17/00
Inventor 王一涛万建波张庆文
Owner UNIVERSITY OF MACAU
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