Method for determining content of mono-ester aconitum alkaloids in ephedra-aconitum carmichaelii-liquorice preparation

A monoester-type alkaloid and determination method technology, which is applied in the field of pharmaceuticals, can solve the problems of low precision and achieve the effects of good durability and improved tailing factor

Active Publication Date: 2015-07-22
SHANDONG TIANSHUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is low precision

Method used

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  • Method for determining content of mono-ester aconitum alkaloids in ephedra-aconitum carmichaelii-liquorice preparation
  • Method for determining content of mono-ester aconitum alkaloids in ephedra-aconitum carmichaelii-liquorice preparation
  • Method for determining content of mono-ester aconitum alkaloids in ephedra-aconitum carmichaelii-liquorice preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0100] Example 1: Determination of Monoester Alkaloid Content in Mafugan Granules

[0101] 1) Preparation of granules:

[0102] 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.

[0103] 2) Content determination:

[0104] Chromatographic conditions and system suitability test: the chromatographic column is filled with polar ether-linked phenyl-bonded silica gel (Welch Ultimate Phenyl-Ether, 250×4.6mm, 5μm, new column); acetonitrile: 0.05% phosphoric acid solution (18: 82) is the mobile phase, add 0.2ml of triethylamine and 0.1ml of di-n-butylamine for every 1000ml of 0.0...

Embodiment 2

[0111] Embodiment 2: Determination of content of monoester type alkaloids in Mafugan Granules

[0112] 1) Preparation of granules:

[0113] 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.

[0114] 2) Content determination:

[0115] Chromatographic conditions and system suitability test: the chromatographic column is filled with polar ether-linked phenyl-bonded silica gel (Welch Ultimate Phenyl-Ether, 30×2.1mm, 3μm, used for 1 month); acetonitrile: 0.2% phosphoric acid solution ( 25:75) is the mobile phase, in which the phosphoric acid solution contains 0.06% triethylamine...

Embodiment 3

[0122] Embodiment 3: Determination of content of monoester type alkaloids in Mafugan Capsules

[0123] 1) Preparation of capsules:

[0124] 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.

[0125] 2) Content determination:

[0126] Chromatographic conditions and system suitability test: the chromatographic column is filled with polar ether-linked phenyl-bonded silica gel (Agela Venusil XBP Polar-Phenyl, 100×4.6mm, 5μm, new column); acetonitrile: 0.1% phosphoric acid solution (20 : 80) is the mobile phase, in which the phosphoric acid solution contains 0.03% triethylamine and 0.02% di-n-butylami...

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Abstract

The invention provides a method for determining the content of mono-ester aconitum alkaloids in an ephedra-aconitum carmichaelii-liquorice preparation. According to the method, high performance liquid chromatography is used for determining the content of mono-ester aconitum alkaloids, a chromatographic column taking polar ether connected phenyl bonded silica gel as filler, and acetonitrile and 0.05-0.2% phosphoric acid solution which are in a ratio of (19:81)-(25:75) are taken as flowing phases, wherein the phosphoric acid solution comprises 0.02%-0.06% of triethylamine and 0.01-0.03% of di-n-butylamine, the detection wavelength is 222-242nm, the number of theoretical plates is not lower than 6000 if calculated by benzoyl mesaconine peak. The separation degree of target components, peak forms and tailing factors are all improved greatly, and moreover, the specificity, linearity, accuracy, precision and durability are all good.

Description

technical field [0001] The invention relates to medicines, in particular to a method for determining the content of aconite alkaloids in Mafugan preparations, belonging to the technical field of medicines. technical background [0002] 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. [0003] Modern studies have shown that monoester alkaloids (benzoyl neoaconitine, benzoyl aconitine, benzoyl hypoaconitine) are both active ingredients and toxic ingredients, and their content must be accurately determined , otherwise its safety and effectiveness cannot be guaranteed. There are many methods for determining the content of monoester-type alkaloids disclosed, but none of them are suitable for the determination of the Mafugan drug, and the effectiveness and safety of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 刘金磊石红艳张为胜李诗标赵颖
Owner SHANDONG TIANSHUN PHARMA
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