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Method for preparing high purity irisquinone, pallason A

A technique for rinsin and gallinin, which is applied in the field of preparing high-purity gallinin, can solve the problems of high difficulty, expensive reagents, long total synthesis route, etc., and achieves avoiding high temperature, reasonable mobile phase components, and expanding sample volume. Effect

Active Publication Date: 2009-11-11
SHANDONG XINHUA PHARMA CO LTD
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  • Abstract
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Problems solved by technology

The total synthetic route is relatively long, the reagents are relatively expensive and difficult
[0010] The preparation of high-purity echinacea by reversed-phase preparative chromatography has not been reported so far

Method used

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  • Method for preparing high purity irisquinone, pallason A
  • Method for preparing high purity irisquinone, pallason A

Examples

Experimental program
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Effect test

preparation example Construction

[0027] The preparation process (known technology) of Radix Iris extract:

[0028] Grind the seed coats of the seeds of Sinus cuspidatum, extract with ethyl acetate reflux, filter, control the temperature of the filtrate below 60°C, concentrate to dryness under reduced pressure at a pressure of -0.07~-0.09MPa, dissolve with ethanol at room temperature, and use an aluminum oxide column layer Analysis, ethanol elution. The temperature of the eluent was controlled below 60°C, concentrated under reduced pressure at -0.07 to -0.09 MPa to 1 / 2 of the original volume, frozen and crystallized at -20°C, and filtered to obtain the crude product. The crude product is recrystallized repeatedly through petroleum ether and ethanol (dissolved at 50°C, crystallized at -20°C) to obtain the extract of Scutellaria radix, of which 83% to 86% (W / W) of sargastin and 9% to 12% of sagerin (W / W).

[0029] Preparation of irinatin solution for preparation:

[0030] The extract of Sciatica japonica was ...

Embodiment 1

[0034] Components for loading samples: irinatin solution for preparation (containing irinatin A 83%, irinatin B 12%)

[0035] Stationary phase: silica gel with octadecyl (C18) ligand

[0036] Column: Luna chromatographic column of Phenomenex Company, 250×10mm

[0037] Flow rate: 5mL / min

[0038] Temperature: 20°C-30°C

[0039] Detection wavelength: 270nm

[0040] Mobile phase: 95% (v / v) acetonitrile in water

[0041] Collect the eluted fractions of peak A, crystallize at minus 20±5°C for 24 hours, filter, and wash three times with acetonitrile at minus 20±5°C. Phosphorus pentoxide is used as desiccant and dried under reduced pressure at room temperature to constant weight. Descaloidin A, the content determined by HPLC method is 99% (area normalization method).

Embodiment 2

[0043] Loading components: erazin solution for preparation (containing 85% elizatin, 9% elizatin B)

[0044] Stationary phase: silica gel with octadecyl (C18) ligand

[0045] Column: Jupiter chromatographic column of Phenomenex Company, 250×25mm

[0046] Flow rate: 10mL / min

[0047] Temperature: 20°C-30°C

[0048] Detection wavelength: 270nm

[0049] Mobile phase: 97% (v / v) acetonitrile in water

[0050] Collect the eluted fraction of peak A, crystallize at minus 20°C to minus 25°C for 24 hours, and filter. Wash three times with cold acetonitrile. Phosphorus pentoxide is used as desiccant and dried under reduced pressure at room temperature to constant weight. Descaloidin A, the content determined by HPLC method is 99% (area normalization method).

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Abstract

The invention provides a method for preparing high purity irisquinone, pallason A, which is characterized in that: the method adopts a reverse phase preparative chromatography, and comprises elution in a liquid chromatography column and a post treatment process of eluted component parts, wherein the elution conditions are that: a sample is irisquinone solution for the preparation, and prepared from Chinese iris seed extract through dissolution by ethanol and acetonitrile, crystallization and filtration respectively; a mobile phase is water-containing acetonitrile solution; the temperature is between 20 and 30 DEG C; and the post treatment process is to crystallize, filter, wash and dry the eluted component parts containing the irisquinone, pallason A after the elution to prepare the high purity irisquinone, pallason A. The method has the characteristics of high purity of prepared products and simple and easy operation.

Description

technical field [0001] The invention relates to the field of pharmacy, in particular to the preparation of high-purity echinacea by reversed-phase preparative chromatography. Background technique [0002] Irisin is the main anti-cancer active ingredient extracted from Iridaceae plant Iris, mainly containing irisin A and irisinin B. [0003] The structure of echinacein (I) is: [0004] [0005] The structure of echinacea (II) is: [0006] [0007] Irinzisu is a Class II new drug of western medicine jointly developed by Shandong Xinhua Pharmaceutical Co., Ltd. and Tianjin Institute of Medical Sciences. It was launched in 1996 and is clinically used as a radiosensitizer in combination with radiotherapy. [0008] The structures of ejaculin and irinzae B are similar, so it is not easy to separate and measure them. Reported HPLC method for the separation and determination of echinacin components: Journal of Pharmaceutical Analysis, 10(4), 1990, P230-232. The provided met...

Claims

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Application Information

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IPC IPC(8): C07C50/28C07C46/10B01D15/08A61P35/00
Inventor 刘怀林孙太红王剑平赵丽
Owner SHANDONG XINHUA PHARMA CO LTD
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