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Method for simultaneously determining three alkaloids in granules for eliminating phlegm and stopping cough for children

A technology for resolving phlegm, relieving cough, and measuring methods, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve the problems of unchecked determination of epecoline and emetine, poor accuracy, environmental pollution, etc., and achieve separation Good, fast filtration speed, less impurity components

Active Publication Date: 2012-09-12
JING JING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the method is cumbersome, time-consuming, pollutes the environment, and has poor accuracy
So far, there is no report on the determination of emetine and emetine by HPLC

Method used

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  • Method for simultaneously determining three alkaloids in granules for eliminating phlegm and stopping cough for children
  • Method for simultaneously determining three alkaloids in granules for eliminating phlegm and stopping cough for children
  • Method for simultaneously determining three alkaloids in granules for eliminating phlegm and stopping cough for children

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Chromatographic conditions and system suitability test Acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 1.5:12.5:86 was used as the mobile phase; column temperature: 40°C; detection wavelength was 205nm; the number of theoretical plates was calculated according to the emetine peak Should not be less than 1200;

[0038] 2. Preparation of reference substance solution Take appropriate amount of ephedrine hydrochloride, emetecine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make stock solution, then take the stock solution, add mobile phase to prepare Become the solution that every 1ml contains ephedrine hydrochloride 50 μ g, emetylline hydrochloride and emetine hydrochloride respectively 4 μ g, to obtain final product;

[0039] 3. Preparation of the test solution Take an appropriate amount of this product, grind it finely, weigh 1 / 2 of the packaged amount of 3g ...

Embodiment 2

[0042] 1. Chromatographic conditions and system suitability test: Acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 2:11.5:86.5 is used as the mobile phase; column temperature: 40°C; detection wavelength is 205nm; the number of theoretical plates is calculated according to the emetine peak Should not be less than 1200;

[0043] 2. Preparation of reference substance solution Take appropriate amount of ephedrine hydrochloride, emetecine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make stock solution, then take the stock solution, add mobile phase to prepare Become the solution that every 1ml contains ephedrine hydrochloride 50 μ g, emetylline hydrochloride and emetine hydrochloride respectively 4 μ g, to obtain final product;

[0044] 3. Preparation of the test solution Take an appropriate amount of this product, grind it finely, weigh 1 / 2 of the packaged amount of 4g pe...

Embodiment 3

[0047] 1. Chromatographic conditions and system suitability test: Acetonitrile-methanol-0.1% phosphoric acid with a volume ratio of 1.0:12.5~11:86.5 is used as the mobile phase; column temperature: 40°C; detection wavelength is 205nm; the number of theoretical plates is based on emetine Peak calculation should not be lower than 1200;

[0048] 2. Preparation of reference substance solution Take appropriate amount of ephedrine hydrochloride, emetecine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make stock solution, then take the stock solution, add mobile phase to prepare Become the solution that every 1ml contains ephedrine hydrochloride 50 μ g, emetylline hydrochloride and emetine hydrochloride respectively 4 μ g, to obtain final product;

[0049] 3. Preparation of the test solution Take an appropriate amount of this product, grind it finely, weigh 1 / 2 of the packaging volume of 5g pe...

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Abstract

The invention relates to a method for simultaneously determining three alkaloids in granules for eliminating the phlegm and stopping the cough for children. The method is characterized in that the HPLC (High Performance Liquid Chromatography) method is employed for the first time, an ordinary gradient elution and reversed-phase chromatographic column are adopted, and acetonitrile, methanol and 0.1% phosphoric acid in the volume ratio of (1.5-2.5) : (12.5-11) : (86-86.5) are taken as the mobile phase; the detection wavelength is 205 nm; and the contents of ephedrine hydrochloride, cephaeline hydrochloride and emetine hydrochloride in the granules for eliminating the phlegm and stopping the cough for children are determined simultaneously, so as to end the history of no HPLC determining method for emetine and no quantitative determining indexes for granules for eliminating the phlegm and stopping the cough for children. The method provided by the invention comprises the steps of performing an ultrasonic treatment to a sample with methanol, sucking a certain amount of subsequent filtrate, removing impurities with an alumina column, and determining. The method has the benefits that crest separation of the three alkaloids is excellent, the baseline is stable, and 30 min is required to finish the determining; the quality control aim of being simple, convenient, quick, scientific, standard and multi-component quantitive by one maker is realized; and safety and effectiveness of taking granules for eliminating the phlegm and stopping the cough for children are ensured.

Description

technical field [0001] The invention relates to a simultaneous determination method of three alkaloids in Xiaoer Huatan Zhike Granules. Background technique [0002] Xiaoer Huatan Zhike Granules is a variety recorded in the ninth volume of the Ministry of Standards, standard number: WS 3 -B-1691-94. It consists of 10ml of Platycodon grandiflora fluid extract, 15ml of Morus alba fluid extract, 3ml of ipecac fluid extract, and 0.375g of ephedrine hydrochloride. It has the effect of eliminating phlegm and relieving cough, and it is used for children. For children with cough, bronchitis. There are dozens of manufacturers of this preparation in the country, and there are currently 3 specifications. The preparation method is as follows: according to the prescription amount, the aqueous solution of Platycodon grandiflora fluid extract, Morus alba fluid extract, ipecac fluid extract, ephedrine hydrochloride, 0.208 g of citric acid and 2.08 g of sodium citrate are sequentially A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89G01N30/12
Inventor 韩桂茹贾永鑫封淑华
Owner JING JING PHARMA
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