Method for extracting glaucocalyxin A

A technology of indigo calyxine and an extraction method, applied in the field of preparing high-purity indigo calyxine, can solve problems such as non-compliance with pharmacopoeia requirements, affecting the use of indigo calyxine, and achieve high purity, strong reproducibility, and yield high effect

Inactive Publication Date: 2010-12-15
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purity of cyanine A obtained by adopting the above-mentioned technical scheme is generally more than 90%, but the yield is generally 7% to 9%, and toxic solvents such as

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 10kg of the above-ground part of blue calyx fragrant tea, crush it, and use 75% ethanol to reflux extraction twice in the normal pressure reflux extraction device, each time reflux extraction for 2 hours, combine the extracts, recover the solvent under reduced pressure, concentrate the extracts, and concentrate The final volume is 3300 milliliters, add 1650 grams of silica gel and stir evenly, dry under reduced pressure, carry out silica gel column chromatography; Silica gel column volume is 17600 milliliters, with 52800 milliliters of sherwood oil: ethyl acetate 8: 1 elution fat-soluble pigment, then The impurities were eluted with 105600 ml of petroleum ether: ethyl acetate 4: 1, and finally eluted with 264000 ml of petroleum ether: ethyl acetate 2: 1. The eluate was collected, concentrated to 20 ml, placed, crystallized, and finally Recrystallized with 20 ml of absolute ethanol to obtain 1.5 g of echinacein A with a purity of 96.0% and a yield of 15%. According t...

Embodiment 2

[0022] Take 10kg of the above-ground part of blue calyx fragrant tea, crush it, and use 80% ethanol to reflux extract 3 times in the normal pressure reflux extraction device, each time reflux extraction for 3 hours, combine the extracts, recover the solvent under reduced pressure, concentrate the extracts, and concentrate The final volume is 3250 milliliters, add 1600 grams of silica gel and stir evenly, dry under reduced pressure, carry out silica gel column chromatography; Silica gel column volume is 18000 milliliters, with 54000 milliliters of sherwood oil: ethyl acetate 8: 1 elution fat-soluble pigment, again Impurities were eluted with 108,000 ml of petroleum ether: ethyl acetate 4:1, and finally eluted with 270,000 ml of petroleum ether: ethyl acetate 2:1. The eluate was collected, concentrated to 20 ml, placed, crystallized, and finally Recrystallized with 20 ml of absolute ethanol to obtain 1.4 g of echinacein A with a purity of 95.6% and a yield of 14%. According to th...

Embodiment 3

[0025] Take 1 kg of the above-ground part of the blue calyx fragrant tea vegetable, crush it, and use 85% ethanol to reflux extract twice in the normal pressure reflux extraction device, each time reflux extraction for 2 hours, combine the extracts, recover the solvent under reduced pressure, concentrate the extracts, concentrate The final volume was 250 milliliters, first extracted three times with an equal volume of petroleum ether, the petroleum ether layer was discarded, and the aqueous layer was extracted three times with an equal volume of chloroform, the combined chloroform layers were concentrated to 10 milliliters, 20 grams of silica gel was added and stirred evenly, and the Dry under pressure, carry out silica gel column chromatography; elute with chloroform:methanol 200:1, compare with thin-layer chromatography, collect the eluate containing cyanine, recover the solvent from the eluate, repeat crystallization with absolute ethanol, Obtained 0.07 g of cyanine A with a...

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PUM

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Abstract

The invention belongs to the field of extraction of traditional Chinese medicines, and in particular relates to a method for preparing high-purity glaucocalyxin A from rabdosia japonica var. galaucocalyx serving as a medicinal material. The method comprises the following steps of: (1) collecting and crushing over-ground part of the rabdosia japonica var. galaucocalyx serving as the raw medicinal material, refluxing and extracting for 2 to 3 times with 75 to 80 percent aqueous solution of ethanol under normal pressure, 2 to 3 hours every time, combining extract, and recovering a solvent under reduced pressure to obtain concentrated extract; (2) adding silica gel into the concentrated extract obtained by the step (1), uniformly stirring the mixture, drying the mixture under reduced pressureand performing silica gel column chromatography; and (3) recrystallizing anhydrous alcohol to obtain the glaucocalyxin A. The glaucocalyxin A obtained by the method has high purity of 95 to 100 percent, is suitable to be prepared into various formulations and has high yield of over 10 percent; and the method has the advantages of high repeatability, no organic solvent residue measured by an organic solvent residue measurement method in pharmacopoeia appendix 2010, no toxicity of suitable organic solvent and conformance to the requirements of the pharmacopoeia 2010.

Description

technical field [0001] The invention belongs to the field of extraction of traditional Chinese medicines, and in particular relates to a method for preparing high-purity cyanine A by using the medicinal materials of calyx calyx and tea leaves as raw materials. Background technique [0002] Eleculin A is the active ingredient of Elysium calyx, which has significant pharmacological activity. Eleculin A can inhibit the production of platelet activating factor by calcimycin-stimulated rabbit platelets, and can inhibit the induction of arachidonic acid. The production of thromboxane A2 in rabbit platelets and the increase of prostaglandin E2 at the same time can significantly inhibit the aggregation of rabbit platelets induced by ADP, AA, PAF, etc., and significantly increase the level of cAMP in platelets (see: Zhang B, Long K. Effects of glaucocalyxin A on aggregation and cAMP levels of rabbit platelets in vitro. Acta Pharmacologica Sinica 1993, 14(4): 347.) Cyclocalyptin has c...

Claims

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Application Information

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IPC IPC(8): C07C49/743C07C45/79
Inventor 张健徐乃玉沈晓丹吴双庆孙群
Owner SUZHOU UNIV
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