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A method for determining the content of diester-type alkaloids of Mafugan medicine

A technology of a diester type alkaloid and a determination method, which is applied in the pharmaceutical field, can solve the problems of low precision, low limit control sensitivity, weak separation ability, etc., and achieves the effects of good durability, improved tailing factor and elimination of interference.

Active Publication Date: 2017-01-18
SHANDONG TIANSHUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can analyze multiple samples at the same time, the amount of developer is small, there are many choices, and the sample processing is simple; the disadvantages are low precision, low limit control sensitivity, and poor repeatability
[0008] High-efficiency capillary electrophoresis: This method has the advantages of short separation time, less interference from impurities, less use of organic solvents, and easy operation; the separation ability is weak, the pH value is high, and the reproducibility is poor

Method used

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  • A method for determining the content of diester-type alkaloids of Mafugan medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Example 1: Determination of Diester Type Alkaloid Content in Mafugan Granules

[0078] 1) Preparation of granules:

[0079] Take 6 kg of aconite, 2 kg of ephedra, and 2 kg of licorice, add water to decoct twice, add 8 times the amount of water for the first time, decoct for 2 hours, add 6 times the amount of water for the second time, decoct for 1 hour, combine the two decoctions, Filter, concentrate to a thick paste, dry under reduced pressure below 80°C, pulverize, mix with appropriate amount of dextrin, make granules, dry, and granulate to obtain the granules of Mafugan drug.

[0080] 2) Content determination:

[0081] The chromatographic conditions and system suitability test used octadecylsilane bonded silica gel as the filler; acetonitrile: tetrahydrofuran (20:20) as the mobile phase A, and 0.01mol / L potassium dihydrogen phosphate solution containing 0.02% phosphoric acid as the Mobile phase B; carry out gradient elution as specified in the table below; the dete...

Embodiment 2

[0089] Embodiment 2: Determination of content of diester type alkaloids in Mafugan Granules

[0090] 1) Preparation of granules:

[0091] Take 12kg aconite, 10kg ephedra, and 10kg licorice, add water to decoct twice, add 10 times the amount of water for the first time, decoct for 2.5 hours, add 8 times the amount of water for the second time, decoct for 1.5 hours, combine the two decoctions, Filter, concentrate to a thick paste, dry under reduced pressure below 80°C, pulverize, mix with appropriate amount of dextrin, make granules, dry, and granulate to obtain the granules of Mafugan drug.

[0092] 2) Content determination:

[0093] Chromatographic conditions and system suitability test using octadecylsilane bonded silica gel as filler; acetonitrile: tetrahydrofuran (30:10) as mobile phase A, 0.05mol / L potassium dihydrogen phosphate solution containing 0.3% phosphoric acid as Mobile phase B; carry out gradient elution as specified in the table below; the detection wavelength i...

Embodiment 3

[0101] Example 3: Determination of Diester Type Alkaloid Content in Mafugan Capsules

[0102] 1) Preparation of capsules:

[0103] Take 10kg aconite, 6.67kg ephedra, and 6.67kg licorice, add water to decoct twice, add 8 times the amount for the first time, decoct for 3 hours, add 6 times the amount for the second time, decoct for 2 hours, filter the decoction, and the filtrate Combined, concentrated to a thick paste, dried under reduced pressure below 80°C, pulverized, mixed with an appropriate amount of starch, packed into capsules to obtain Mafugan capsules.

[0104] 2) Content determination:

[0105] Chromatographic conditions and system suitability test using octadecylsilane bonded silica gel as filler; acetonitrile: tetrahydrofuran (26:14) as mobile phase A, 0.04mol / L potassium dihydrogen phosphate solution containing 0.1% phosphoric acid as Mobile phase B; carry out gradient elution as specified in the table below; the detection wavelength is 230nm; the number of theor...

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Abstract

The invention provides a method for determining the content of diester-type alkaloids in an ephedra-monkshood-radix glycyrrhizae medicament. The method is implemented by using high performance liquid chromatography, and a chromatographic column takes octadecylsilane chemically bonded silica as a filler; and by taking acetonitrile-tetrahydrofuran as a mobile phase A and a phosphoric acid solution (including potassium dihydrogen phosphate) as a mobile phase B, programmed gradient elution is performed by time, and determination is performed by using a sample-reference substance mixed method, the separating degree, peak shape and tailing factor of a target component are significantly improved, and the specificity, recovery, precision and durability of the target component are good.

Description

technical field [0001] The invention relates to medicines, in particular to a method for determining the content of aconite alkaloids in Mafugan medicine, and belongs to the technical field of medicines. [0002] technical background [0003] Mafugan Preparation is the abbreviation of Mahuang Fuzi Gancao Decoction, which is composed of Fuzi, Ephedra, and Licorice. Its prescription comes from "Treatise on Febrile Diseases". , aversion to cold and body pain, no sweat, slight fever, deep and weak pulse. [0004] The alkaloids contained in aconite mainly include diester alkaloids, monoester alkaloids and amino alcohol alkaloids. Modern studies have shown that diester-type alkaloids (neaconitine, hypoaconitine, aconitine) are toxic components, and there are many methods for measuring the content of diester-type alkaloids disclosed, but none of them are suitable for the The determination of sweet drugs cannot effectively guarantee the safety of products in production and use. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 方方石红艳赵颖李诗标张为胜
Owner SHANDONG TIANSHUN PHARMA