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Method for extracting and separating kaempferol from impatiens balsamina

A separation method, the technology of kaempferol, applied in the direction of organic chemistry, etc., can solve the problems of limited amount of kaempferol, complex process, expensive dextran gel, etc.

Inactive Publication Date: 2011-01-12
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reasons are: 1) dextran gel (LH-20) is more expensive; 2) the preparation of high-performance liquid phase equipment is expensive, and the amount of kaempferol prepared at the same time is limited
In addition, the method has many steps and the process is more complicated.

Method used

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  • Method for extracting and separating kaempferol from impatiens balsamina

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0035] Experimental Example 1: Purity Check of Kaempferol

[0036] Check the purity by HPLC. Instrument: Waters 600 high performance liquid chromatography. Column: YWG-C 18 Chromatography column, 250mm×4.6mm, 5μm. Mobile phase: methanol-0.1% phosphoric acid aqueous solution (50~70:50~30); flow rate: 0.8~1.2mL / min; column temperature: room temperature; detection wavelength: 367nm; injection volume: 10μl; retention time (RT): Kaempferol: 5-30min; chromatogram recording time: 60min. The area normalization method measures the purity, and the purity of kaempferol is 98.8%.

experiment example 2

[0037] Experimental Example 2: Determination of the structure of kaempferol

[0038] Melting point was measured by X-4 digital display microscopic melting point tester; ultraviolet (UV) spectrum was measured by Japan Shimadzu UV-260 UV-visible spectrophotometer; infrared (IR) spectrum was measured by Perkin-Elmer 983G instrument, KBr tablet ; H NMR and C NMR spectra ( 1 HNMR and 13 CNMR) is measured with MERCURY-400 nuclear magnetic resonance instrument; Mass spectrometry (MS) is measured with Finnigan-LCQ DECA type mass spectrometry.

[0039]The pure kaempferol obtained by the above-mentioned purification method is yellow granular crystal with a melting point of 276-278°C. UVλmax (nm): 226, 267, 349. IRυmax(KBr, cm -1 ): 3324 (OH), 1662 (C=O). MS (m / z): 309 (M+Na). 1 H NMR (δ, DMSO-d 6 ): 12.47 (5-OH), 10.85 (7-OH), 10.12 (3-OH), 9.43 (4'-OH), 8.03 (2H, d, J=9.0 Hz, C 2′ -H,C 6′ -H), 6.91 (2H, d, J=9.0Hz, C 3′ -H,C 5′ -H), 6.43 (1H, d, J=1.8Hz, C 8 -H), 6.18 (1H,...

experiment example 3

[0042] Experimental Example 3 Experiment of macroporous adsorption resin for enriching crude kaempferol

[0043] Take 2.5kg of dried balsam flower petals, add 75L of ethanol with a concentration of 80%, heat and reflux for extraction for 1 hour, filter, extract the medicinal residues successively 3 times by the same method, combine the extracts, and discard the medicinal residues; the extracts are recovered Ethanol to obtain a thick paste that is total extract 0.68kg.

[0044] Take 0.68kg of the above-mentioned total extract, add 15L of water to dilute, use a D101 type macroporous adsorption resin column, the resin amount is 20L (volume in water), the diameter-to-height ratio is 1:6, and the adsorption flow rate is 3BV / h; first wash out 9BV with water , the flow rate is 3BV / h, then 9BV is eluted with 30% ethanol, the flow rate is 3BV / h; finally, the 4BV is eluted with 50% ethanol, the flow rate is 2BV / h, this part of the eluate is collected, and the solvent is recovered to obt...

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Abstract

The invention discloses a method for extracting and separating kaempferol from impatiens balsamina, which relates to a method for extracting and separating active ingredients of traditional Chinese medicaments, in particular to a method for extracting and separating the kaempferol. The method is provided to solve the problems of complicated kaempferol preparation process and high cost of the current kaempferol preparation process. The method comprises the following steps of: firstly, extracting the impatiens balsamina to obtain a total extract; secondly, purifying the total extract by using macroporous resin to obtain a crude kaempferol product; and finally, preparing a pure kaempferol product by using a column chromatography and re-crystallization method. The method can effectively separate the kaempferol monomer from the impatiens balsamina, provides a reference product for performing the quality detection of Chinese medicaments containing the kaempferol and is favorable for developing the activities of the kaempferol.

Description

technical field [0001] The invention relates to a method for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating kaempferol. Background technique [0002] Kaempferol is a flavonol compound. The compound has a variety of pharmacological activities, such as anti-oxidation, anti-inflammatory, etc., and exists in a variety of traditional Chinese medicines and their related preparations, such as Ginkgo biloba and its extracts and preparations, mulberry leaves, white stamens, Shiwei, dodder, Mangosteen, Qianqiantonglin granules, etc. The content of kaempferol is an important detection index for the quality of the above-mentioned traditional Chinese medicines and preparations. Therefore, it is necessary to extract kaempferol with high separation purity as a reference substance in practical work. At the same time, kaempferol is a component with various pharmacological activities. In the process of i...

Claims

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Application Information

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IPC IPC(8): C07D311/30C07D311/40
Inventor 姜华李军柴元武刘璐李晓明
Owner HENAN UNIV OF SCI & TECH
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