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Preparation method of Corydalis bungeana reference substance

A technology of Corydalis chinensis and reference substances, which is applied in the field of preparation of solid reference substances, can solve problems such as limitations in application scenarios, and achieve the effects of less process steps, less time-consuming, and high purity

Inactive Publication Date: 2021-06-01
上海诗丹德标准技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Corydalis ling obtained by the existing preparation method and the standard substance that can be bought on the market, although the HPLC purity is acceptable, but when used for TLC qualitative detection, there are impurities in itself, so that the application scene as a reference substance is greatly restricted. big limit

Method used

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  • Preparation method of Corydalis bungeana reference substance
  • Preparation method of Corydalis bungeana reference substance
  • Preparation method of Corydalis bungeana reference substance

Examples

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preparation example Construction

[0040] The preparation and separation method of the present invention includes the following steps in sequence: the first normal-phase chromatographic column purification process, loading the concentrated liquid of the extract concentrate of the pulverized medicinal material Kudidin to the normal-phase chromatographic column, and using a liquid containing petroleum ether, ethyl acetate, three Impurities are eluted with a mixed solvent of ethylamine. At this time, the mixing ratio of petroleum ether: ethyl acetate: triethylamine is 3-6: 0.05-0.2: 0.05-0.2. The eluted target substance is concentrated to obtain a crude product concentrate containing the target substance,

[0041] In the insoluble solvent precipitation treatment process, the crude concentrated solution containing the target substance is dissolved in dichloromethane, and then diluted with a mixed solution of dichloromethane:methanol 1.5-0.8:1, and then added For the solvent of soluble solvent, the solution is conce...

Embodiment 1

[0056] Extraction of raw materials: Take 500kg of medicinal materials, add 200L of 90% ethanol (purchased from Shanghai Titan Technology Co., Ltd., 25L / barrel) for each 30kg of medicinal materials for thermal extraction once, recover the solvent for multiple use, concentrate at 60°C to obtain a concentrated solution of 100L, and quantify by HPLC about Contains Corydalin 448g;

[0057] Extraction and impurity removal: add 6% HCl (purchased from Shanghai Titan Technology Co., Ltd., 500ml / bottle) to the concentrated solution to adjust the pH to 2-3, and use an equal volume of petroleum ether (purchased from Shanghai Titan Technology Co., Ltd., 25L / barrel) to extract 3 times, after the extraction, the aqueous layer was adjusted to pH 8-9 with concentrated ammonia water (purchased from Shanghai Titan Technology Co. , 25L / barrel) extracted 1 to 2 times to obtain the ethyl acetate layer, and HPLC quantified that the ethyl acetate layer contained 300 g of Corydalin;

[0058] Silica ...

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Abstract

The invention provides a preparation method of a Corydalis bungeana reference substance. The preparation method comprises a first normal-phase chromatographic column purification process, an insoluble solvent precipitation treatment process and a second normal-phase chromatographic column purification process. The reference substance prepared by the method not only has high HPLC purity, but also has very high TLC purity. In addition, the obtained solid reference substance of the corydalis bungeana is also very excellent in indexes in the aspects of moisture, solvent residues, burning residues and the like.

Description

technical field [0001] The invention relates to a preparation method of cordyline, in particular to a preparation method capable of preparing a solid reference substance that can be used for TCL high-purity cordyline. Background technique [0002] Corydalis bungeana (Corydalis bungeana) is the dried whole herb of Corydalis genus Corydalis in the family Papaveraceae, also known as Xiaojicai, Corydalis pengeana. For the treatment of epidemic cold, sore throat, boils and sores, carbuncle on the back, mumps and erysipelas, decoction of chrysanthemum decoction can play a certain role in daily health care, and it has a certain effect on eliminating toxins and enhancing resistance . [0003] As a quality control method of Kudiding Chinese medicinal material, Corydalin, the main compound specified in the Pharmacopoeia of the People's Republic of China, is its index component. Violet spirit is the main ingredient in Kudiding. Corynoline, the molecular formula is C 21 h 21 NO 5 ...

Claims

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Application Information

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IPC IPC(8): C07D491/153
CPCC07D491/153
Inventor 李雪松丁云吴佳卢宗元钱勇谢天培
Owner 上海诗丹德标准技术服务有限公司
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