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Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method

A technology for active ingredients and determination methods, which is applied in the field of quality control of medicinal materials and their preparations, and can solve problems such as the lack of specificity of quercetin

Inactive Publication Date: 2010-10-06
GUIZHOU NORMAL UNIVERSITY
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AI Technical Summary

Problems solved by technology

The 2010 edition of "Chinese Pharmacopoeia" included the medicinal materials of Quercetin. In this standard, the quality control of the medicinal materials of Quercetin was carried out by measuring the content of quercetin. However, the specificity of quercetin is not strong, and many herbal medicinal materials contain quercetin. Therefore, in order to make the clinical application of Ganbangui more safe, effective, scientific and reasonable, its quality control must be strengthened and a more reasonable quality control method must be formulated

Method used

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  • Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method
  • Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method
  • Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method

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Experimental program
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Effect test

Embodiment 1

[0086] Embodiment 1 of the present invention: the preparation method of the reference substance of the active ingredient in the medicinal material of Gossypium chinensis (see figure 1 ): Dried and pulverized the medicinal materials of the ganglion, and extracted 3 times with 75% ethanol under reflux, evaporated the solvent to obtain the extract, dispersed the extract with water, and then extracted with ethyl acetate and n-butanol, and the ethyl acetate part was repeatedly subjected to silica gel column Chromatography, gradient elution with chloroform-methanol, chloroform-methanol=30:1 part of the extract was concentrated to obtain methyl p-coumarate reference substance; chloroform-methanol=20:1 part of the extract was concentrated to obtain 5-hydroxymethyl Furfural reference substance; n-butanol part is repeatedly subjected to silica gel column chromatography, gradient elution with chloroform-methanol, chloroform-methanol=10:1 part of the extract is concentrated, and quercetin...

Embodiment 2

[0087] Embodiment 2 of the present invention: Quercetin-3-O in the medicinal materials -β- Determination method of D-glucuronic acid: Determination by high performance liquid chromatography according to Appendix VID of "Chinese Pharmacopoeia" 2010 Edition:

[0088] Chromatographic conditions and system suitability test: use octadecyl-bonded silica gel as filler; use methanol-aqueous solution of phosphoric acid with a mass concentration of 0.05% (43∶57) as mobile phase; flow rate 1.0mL·min -1 ; The column temperature is 30 °C; the detection wavelength is 258 nm; the theoretical plate number is based on quercetin-3-O -β- D-glucuronic acid peak calculation should not be less than 3000;

[0089] Preparation of reference solution: precise weighing of quercetin-3-O -β- An appropriate amount of D-glucuronic acid reference substance (prepared in Example 1) was added with methanol to make a solution containing 0.1 mg per 1 mL, that is;

[0090] Preparation of the test solution: take...

Embodiment 3

[0093] Embodiment 3 of the present invention: Quercetin-3-O in the medicinal materials -β- Determination method of D-glucuronic acid: Determination by high performance liquid chromatography according to Appendix VID of "Chinese Pharmacopoeia" 2010 Edition:

[0094] Chromatographic conditions and system suitability test: use octadecyl-bonded silica gel as filler; use methanol-0.06% phosphoric acid aqueous solution (40∶60) as mobile phase; flow rate 1.0mL·min -1 ; The column temperature is 25°C; the detection wavelength is 260 nm; the theoretical plate number is based on quercetin-3-O -β-D-glucuronic acid peak calculation should not be less than 3000;

[0095] Preparation of reference solution: accurately weigh quercetin-3-O -β- Add appropriate amount of D-glucuronic acid reference substance (made by the applicant), add methanol to make a solution containing 0.01mg per 1mL, and obtain it;

[0096] Preparation of the test solution: take 0.2 g of the powder of the barbaric medi...

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Abstract

The invention discloses a polygonum perfoliatum medicinal material, a method for preparing a reference substance of active constituents in a preparation thereof as well as a content determination method. The content determination method adopts a high efficiency liquid chromatography to determine contents of quercetin-3-O-belta-D-glucuronic acid and the like contained in the polygonum perfoliatum medicinal material and the preparation thereof in the same chromatographic condition. Compared with the prior art, the content determination method for determining the contents of quercetin-3-O-belta-D-glucuronic acid and the like contained in the polygonum perfoliatum medicinal material and the preparation thereof is created to improve the quality detection standard of the polygonum perfoliatum medicinal material and the preparation thereof and make up the deficiency of the traditional quality control technique, and the quality control technique for the polygonum perfoliatum medicinal material and the preparation thereof is more scientific and reasonable. The content determination method has the advantages of high precision, good repeatability, high stability, high recovery rate and accurate measuring result. The content determination method can effectively control the quality of the polygonum perfoliatum medicinal material and the preparation thereof so as to ensure safety and effectiveness in clinical application.

Description

technical field [0001] The invention relates to a preparation method and a content determination method for a reference substance of the active ingredient in the medicinal material and the preparation thereof, and belongs to the technical field of quality control of the medicinal material and the preparation thereof. Background technique [0002] Most of the traditional Chinese medicines and their preparations in my country lack strict quality standards and scientific testing methods, so it is difficult to effectively control their internal quality, cannot guarantee the safety and effectiveness of medication, and do not meet the requirements of the international pharmaceutical market, which seriously restricts the Chinese medicine industry in my country. development of. Strengthening the research on the quality control of traditional Chinese medicinal materials is a key issue in the standardization and standardization of traditional Chinese medicine. Only by carrying out sci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08C07C69/732C07C67/48C07D307/46G01N30/02G01N30/36
Inventor 周欣陈华国赵超龚小见范东生
Owner GUIZHOU NORMAL UNIVERSITY
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