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Method for adopting pH gradient elution method to synchronously separate triterpenoid saponins and licorice flavonoid

A triterpenoid saponins and synchronous separation technology, applied in the field of chemical compounds, can solve the problems of high energy consumption and ethanol consumption of solvent recovery, and achieve the effects of full utilization, reduction of consumption, and production cost savings

Active Publication Date: 2015-09-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to change the current situation that the traditional macroporous resin ethanol elution process consumes more ethanol and the energy consumption of solvent recovery is large, and uses the extract after extracting polysaccharides from licorice as raw material, and utilizes triterpenoid saponins and licorice flavonoids In order to improve the yield of target components and save production costs, alkaline solution is preferred as the elution solvent for gradient separation to improve the yield of target components and save production costs; at the same time, according to the characteristics of glycyrrhizic acid being easily soluble in hot water, and heating in chemical, chemical and pharmaceutical processes In favor of the principle of mass transfer, a high borosilicate glass interlayer chromatography column with controllable column temperature was designed and developed and used in the elution process, which can be eluted under heating conditions to increase the yield of glycyrrhizic acid and realize the licorice The full and effective use of resources also provides a simple and easy experimental device for the very temperature column separation of temperature-sensitive special components in the fields of chemistry, chemical industry and pharmaceuticals

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  • Method for adopting pH gradient elution method to synchronously separate triterpenoid saponins and licorice flavonoid
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Embodiment 1

[0036] The pH gradient elution method of the present invention is applied to the process technology and equipment for synchronously separating triterpene saponins and licorice flavonoids in licorice paste, including the following steps:

[0037] 1. Preparation of loading solution

[0038] The licorice fluid extract to be recycled after extracting polysaccharides was stirred and dissolved with purified water at room temperature (fluid extract:purified water volume ratio 1:4), centrifuged for 20min (speed 4000r / min), and the supernatant was prepared into a suitable concentration as the loading solution.

[0039] 2. Pretreatment of macroporous resin

[0040]Soak the pharmaceutical-grade resin HPD100, which was optimized by the static adsorption and elution experiment, in ethanol for 24 hours, then wash the resin with a large amount of purified water until it has no alcohol smell, and soak it in water for later use.

[0041] 3. Sample loading and adsorption: Accurately weigh the...

Embodiment 2

[0046] The pH gradient elution method of the present invention is applied to the process technology and equipment for synchronously separating triterpene saponins and licorice flavonoids in licorice paste, including the following steps:

[0047] 1. Preparation of loading solution

[0048] The licorice fluid extract to be recycled after extracting polysaccharides was stirred and dissolved with purified water at room temperature (fluid extract:purified water volume ratio 1:4), centrifuged for 20min (speed 4000r / min), and the supernatant was prepared into a suitable concentration as the loading solution.

[0049] 2. Pretreatment of macroporous resin

[0050] Soak the pharmaceutical-grade resin HPD400, which was optimized by the static adsorption and elution experiment, in ethanol for 24 hours, then wash the resin with a large amount of purified water until it has no alcohol smell, and soak it in water for later use.

[0051] 3. Sample loading and adsorption: Accurately weigh th...

Embodiment 3

[0056] The pH gradient elution method of the present invention is applied to the process technology and equipment for synchronously separating triterpene saponins and licorice flavonoids in licorice paste, including the following steps:

[0057] 1. Preparation of loading solution

[0058] The licorice fluid extract to be recycled after extracting polysaccharides was stirred and dissolved with purified water at room temperature (fluid extract:purified water volume ratio 1:4), centrifuged for 20min (speed 4000r / min), and the supernatant was prepared into a suitable concentration as the loading solution.

[0059] 2. Pretreatment of macroporous resin

[0060] Soak the pharmaceutical-grade resin HPD450, which was optimized by the static adsorption and elution experiment, in ethanol for 24 hours, wash the resin with a large amount of purified water until it has no alcohol smell, and soak it in water for later use.

[0061] 3. Sample loading and adsorption: Accurately weigh the pre...

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Abstract

The invention relates to a method for adopting a pH gradient elution method to synchronously separate triterpenoid saponins and licorice flavonoid. Eluent taking triterpenoid saponins as a main ingredient and eluent containing licorice flavonoid and other useful ingredients are obtained respectively through preparation of a sample loading solution, pretreatment of macroporous resin, loaded sample adsorption, preheating and application interlayer chromatography for pH gradient elution and adopting sodium carbonate solution, sodium bicarbonate solution or sodium hydroxide solution which are different in alkalinity. Yield of glycyrrhizic acid can be increased by 2-4 times when compared with that of a method taking ethanol solution as eluant, ethanol consumption and consumption caused by ethanol recovery are lowered, yield of glycyrrhizic acid can be increased by more than 60% to greatest extent when compared with that of a normal-temperature elution process, an experimental device which is simple, convenient and easy is provided for non-normal-temperature column separation of temperature-sensitive special ingredients in the field of chemistry, chemical engineering and pharmaceuticals, and the method has popularization value.

Description

technical field [0001] The invention relates to a method for synchronously separating compounds such as triterpene saponins and licorice flavonoids in licorice paste by a pH gradient elution method. Background technique [0002] Licorice is the dry root and rhizome of Glycyrrhiza uralensis Fisch, Glycyrrhiza uralensis Fisch, Glycyrrhiza inflata Bat, Glycyrrhiza glabra L, and Glycyrrhiza uralensis Fisch. It is mainly produced in Inner Mongolia, Gansu, Xinjiang, Ningxia and Northeast China. Harvest in spring and autumn, preferably in autumn. Licorice is sweet in taste and flat in nature, and it returns to the heart, lung, spleen, and stomach meridians. It has the effects of invigorating the spleen and replenishing qi, eliminating phlegm and relieving cough, relieving spasm and relieving pain, clearing away heat and detoxification, and harmonizing various medicines. [0003] According to existing data reports, more than 100 kinds of flavonoids, more than 60 kinds of triterpe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/06A61K36/484
CPCA61K36/484C07H1/06C07H15/256C07J63/008
Inventor 刘明言凌宁生见玉娟
Owner TIANJIN UNIV
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