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Preparation method for robinin

A kind of locust glycoside and supercritical technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, and bulk chemical production, etc., can solve the problems such as the lack of reports on the preparation process of high-purity locust glycosides, and achieves the advantages of large-scale production operation and energy efficiency. Low consumption and low pollution

Inactive Publication Date: 2011-02-16
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, there is no report on the preparation process suitable for the industrialized large-scale production of high-purity acacia glycosides

Method used

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  • Preparation method for robinin

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Experimental program
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Effect test

Embodiment 1

[0023] Get 10Kg of Robinia locust leaves, crush them, and add them to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 2%, the extraction pressure is 10MPa, the temperature is 40°C, and CO 2 The flow rate is 1ml / g crude drug min, and the extraction time is 80min to obtain the extract, which is added to the polyamide 6 (polycaprolactam) polyamide column and eluted with ethanol-pyridine mixed solvent with a ratio of 8:1 as the eluent. At the same time, use the same type of polyamide film to develop with the above eluent as a supporting test, collect the fraction corresponding to Rf=4-4.5 on the polyamide film, recover the solvent, concentrate, and add water-pyridine in a ratio of 1:1 The mixed solvent was crystallized, washed and dried to obtain 3.15 g of white needle-like crystals - acaciaside, which was detected by HPLC with a purity of 90.9%, UV, IR, MS, 2 HNMR, 13 The data ch...

Embodiment 2

[0025] Get 10Kg of Robinia locust leaves, crush them, and add them to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 8%, the extraction pressure is 30MPa, the temperature is 55°C, and CO 2 The flow rate is 4ml / g crude drug·min, the extraction time is 200min, and the extract is obtained, which is added to the polyamide chromatographic column of nylon 66 (polyhexamethylene adipamide), and the ethanol-pyridine mixed solvent with a ratio of 8:1 is used as the washing agent. Elution with detaching agent, at the same time, use the same kind of polyamide film to develop with the above eluent as a supporting detection, collect the fraction corresponding to Rf=4-4.5 on the polyamide film, recover the solvent, concentrate, and add the ratio of 1: 1 of water-pyridine mixed solvent crystallized, washed and dried to obtain 3.43 g of white needle-like crystals - acaciaside, which was detecte...

Embodiment 3

[0027] Get 10Kg of Robinia locust leaves, crush them, and add them to CO 2 In the supercritical extractor, ethanol is used as an entrainer, and the volume percentage of the entrainer in the total extraction solvent is 5%, the extraction pressure is 20MPa, the temperature is 45°C, and CO 2 The flow rate is 2ml / g crude drug min, and the extraction time is 150min to obtain the extract, which is added to the polyamide chromatographic column of nylon 6 (polycaprolactam) and eluted with a mixed solvent of ethanol-pyridine in a ratio of 8:1 as the eluent. At the same time, use the same type of polyamide film to develop with the above eluent as a supporting test, collect the fraction corresponding to Rf=4-4.5 on the polyamide film, recover the solvent, concentrate, and add water-pyridine in a ratio of 1:1 The mixed solvent was crystallized, washed and dried to obtain 3.68 g of white needle-like crystals - acaciaside, which was detected by HPLC with a purity of 95.2%, UV, IR, MS, 2 HN...

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Abstract

The invention relates to a preparation method for robinin, which has the advantages of simple and convenient operation, low pollution and less energy consumption. The preparation method comprises the following processing steps: taking robinia leaves, crushing the robinia leaves, adding the crushed robinia leaves into a CO2 supercritical extractor for supercritical extraction, adding the extractedrobinia leaves on a polyamide chromatographic column, taking an alcohol-pyridine mixed solvent with the proportion of 8:1 as an eluant for elution, simultaneously using a similar polyamide film to detect by matching with the eluant, collecting flow component corresponding to Rf=4-4.5 on the polyamide film, recovering the solvent, concentrating the solvent, adding water-pyridine mixed solvent in the proportion of 1:1 for crystallization, washing, drying and obtaining the robinin. The prepared robinin by adopting the method of the invention has high purity, and is easy to realize the industrialamplification.

Description

technical field [0001] The invention relates to a preparation method of acacia glucoside, in particular to a preparation method of extracting acacia glycoside from plants. Background technique [0002] Acaciin (Linarin), molecular formula: C 28 h 32 o 14 , Molecular weight: 592.552, CAS registration number: 480-36-4, exists in various plants of Buddleiaceae, Ranunculaceae, Compositae, and Fabaceae, among which the leaves of Robinia pseudoacacia L., a leguminous plant, are rich in content . Its molecular formula is as follows: [0003] [0004] Modern studies have shown that acacia glycosides have multiple functions such as inhibiting phosphodiesterase, protecting the liver, and treating bronchitis, and it is also used as a raw material for the synthesis of other active derivatives. [0005] In the prior art, there is no report on a preparation process suitable for the industrialized mass production of high-purity acacia glycosides. Contents of the invention [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08
CPCY02P20/54
Inventor 张发成毛志英
Owner 南京璇荣贸易有限公司
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