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Method for separating and purifying Centella asiatica triterpene acid monoglucoside

A technology of monoglucoside and oxatriterpene acid, applied in organic chemistry, steroids, etc., to achieve the effect of being suitable for large-scale production and application, low cost, and simple operation

Inactive Publication Date: 2012-03-07
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no separation and purification of asiatic acid monoglucoside, chebuside II and hydroxy asiatic acid monoglucoside from the crude product of centella asiatic acid monoglucoside. research report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve or suspend 1 g of the asiatic acid monoglucoside composition in 0.5 mL of methanol, and use 30 g of ODS C 18 The semi-preparative liquid chromatography of the column was chromatographed, and the aqueous methanol solution containing 0.05% β-cyclodextrin by mass percentage was used to elute, wherein the volume ratio of methanol:water was 1:2, and cerbutin II and hydroxyl Asiatic acid monoglucoside and asiatic acid monoglucoside fractions, concentrated to dryness under reduced pressure at 40°C, adding 50% methanol aqueous solution, heating and dissolving to a saturated solution, cooling to crystallize, and recrystallizing once to obtain chebuside II. Madecasic acid monoglucoside and asiatic acid monoglucoside.

[0027] The content was determined by HPLC, and the results showed that the mass percent contents of chebuside II, madecasic acid monoglucoside and asiatic acid monoglucoside were 97.6%, 96.3% and 94.1%, respectively.

Embodiment 2

[0029] Dissolve or suspend 10 g of the asiatic acid monoglucoside composition in 50 mL of methanol, and use 2 kg of ODS C 18 The column was chromatographed by a preparative liquid chromatograph, and eluted with aqueous methanol containing 0.4% β-cyclodextrin by mass percentage, wherein the volume ratio of methanol:water was 1:4, and cerbutin II and hydroxyl Asiatic acid monoglucoside and asiatic acid monoglucoside fractions, concentrated to dryness under reduced pressure at 40°C, adding 50% methanol aqueous solution, heating to dissolve into a saturated solution, cooling to crystallize, and recrystallizing twice to obtain chebuside II. Madecasic acid monoglucoside and asiatic acid monoglucoside.

[0030] The content was determined by HPLC, and the results showed that the mass percentages of chebuside II, madecasic acid monoglucoside and asiatic acid monoglucoside were 98.6%, 98.3% and 98.1%, respectively.

Embodiment 3

[0032] Dissolve or suspend 10 g of the asiatic acid monoglucoside composition in 30 mL of methanol, and use a C 18 The preparative liquid chromatography of the column was used for chromatography, and the aqueous ethanol solution containing 0.4% β-cyclodextrin was used for elution, wherein the ethanol:water volume ratio was 1:4, and cerbutin II and hydroxyl Asiatic acid monoglucoside and asiatic acid monoglucoside fractions, concentrated to dryness under reduced pressure at 60°C, adding 50% ethanol aqueous solution, heating and dissolving to a saturated solution, cooling to crystallize, and recrystallizing 3 times to obtain chebuside II. Madecasic acid monoglucoside and asiatic acid monoglucoside.

[0033]Asiatic acid monoglucoside, hydroxyasiatic acid monoglucoside and chebuside II were determined by HPLC, and the mass percent contents were 98.3%, 97.3% and 99.1%, respectively.

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Abstract

The invention discloses a method for separating and purifying Centella asiatica triterpene acid monoglucoside by using crude Centella asiatica triterpene acid monoglucoside as the raw material. The method comprises the following steps: carrying out column chromatography on crude Centella asiatica triterpene acid monoglucoside, eluting using a mobile phase containing beta-cyclodextrin, collecting fractions respectively, and concentrating and drying to obtain asiatic acid monoglucoside, chebuloside II and madecassic acid monoglucoside. By adopting the technical scheme of the invention, pure Centella asiatica triterpene acid monoglucoside can be separated from crude Centella asiatica triterpene acid monoglucoside. In addition, the method is simple to operate, has lower cost and is suitable for large-scale production and applications.

Description

technical field [0001] The invention belongs to the field of natural medicines, and relates to a method for separating and purifying various centella asiatica triterpene acid monoglucosides using crude centella asiatica triterpene acid monoglucoside as raw materials. Background technique [0002] Centella asiatica (L.) Urb, also known as Luodeda, Bengdawan, and Banbianqian, is a plant of the genus Centella asiatica in the family Umbelliferae. It was first recorded in "Shen Nong's Materia Medica" and listed as a middle grade. It is cold in nature, bitter and pungent in taste, and has the effects of clearing heat and promoting dampness, detoxifying and reducing swelling. It is mainly used for damp-heat jaundice, heatstroke diarrhea, sandy and bloody stranguria, carbuncle sores, and traumatic injuries. Centella asiatica is a commonly used Chinese herbal medicine in the Guangdong area. It has a history of more than 2,000 years in our country to use centella asiatica for external...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 茅仁刚宋纯清袁萍叶晓平杜鹏司鹏鹏吴博
Owner SHANGHAI NORMAL UNIVERSITY
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