HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in ipecacuanha medicinal material and preparation of ipecacuanha medicinal material

A technology for ipecacine hydrochloride and ipecacine hydrochloride, which is applied in the field of ipecacine hydrochloride and ipecacine hydrochloride HPLC quantitative analysis, can solve the problems of polluted environment, complicated operation, difficult to guarantee accuracy and the like, and achieves high sensitivity, The effect of reducing pollution and sampling less

Active Publication Date: 2012-08-15
JING JING PHARMA
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  • Abstract
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  • Claims
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Problems solved by technology

The liquid extract of ipecac and tincture of ipecac are raw material preparations attached to the quality standard of Xiaoer Huatan Zhike Granules. The quantitative determination methods are acid dissolution, chloroform extraction to remove impurities, alkalization, chloroform extraction of alkaloids, steaming Dry, acid-base titration, cumbersome operation, pollutes the environment, and the accuracy is difficult to guarantee

Method used

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  • HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in ipecacuanha medicinal material and preparation of ipecacuanha medicinal material
  • HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in ipecacuanha medicinal material and preparation of ipecacuanha medicinal material
  • HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in ipecacuanha medicinal material and preparation of ipecacuanha medicinal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: Quantitative method of emetenyl hydrochloride and emetine HPLC in the medicinal material of ipecac

[0044] (1) Chromatographic conditions and system suitability test take acetonitrile-methanol-0.1% phosphoric acid as the mobile phase with a volume ratio of 9:3:88; column temperature: 40°C; detection wavelength is 205nm; the number of theoretical plates is based on emetine hydrochloride Peak calculation should not be lower than 1500;

[0045] (2) Preparation of Reference Substance Solution Take an appropriate amount of emetine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make the stock solution, then take the stock solution, add mobile phase to make 1ml A solution containing 10-30 μg of emetine hydrochloride and 30-10 μg of emetine hydrochloride;

[0046] (3) Preparation of the test solution: Take 0.1 g of the fine powder of ipecac medicinal material, accurately w...

Embodiment 2

[0048] Embodiment 2: HPLC quantitative method of emetine hydrochloride and emetine in the liquid extract of ipecac

[0049] (1) Chromatographic conditions and system suitability test take acetonitrile-methanol-0.1% phosphoric acid as the mobile phase with a volume ratio of 8.5:4:87.5; column temperature: 40°C; detection wavelength is 205nm; the number of theoretical plates is based on emetine hydrochloride Peak calculation should not be lower than 1500;

[0050] (2) Preparation of Reference Substance Solution Take an appropriate amount of emetine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make the stock solution, then take the stock solution, add mobile phase to make 1ml A solution containing 10-30 μg of emetine hydrochloride and 30-10 μg of emetine hydrochloride;

[0051] (3) Preparation of the test solution Precisely draw 1ml of ipecac liquid extract, put it in a 25ml measuring bo...

Embodiment 3

[0053] Embodiment 3: HPLC quantitative method of emetenyl hydrochloride and emetine in ipecac tincture

[0054] (1) Chromatographic conditions and system suitability test take acetonitrile-methanol-0.1% phosphoric acid as the mobile phase with a volume ratio of 9.5:3.1:87.4; column temperature: 40°C; detection wavelength is 205nm; the number of theoretical plates is based on emetine hydrochloride Peak calculation should not be lower than 1500;

[0055] (2) Preparation of Reference Substance Solution Take an appropriate amount of emetine hydrochloride and emetine hydrochloride reference substance, accurately weigh them, put them in a brown measuring bottle, add methanol to make the stock solution, then take the stock solution, add mobile phase to make 1ml A solution containing 10-30 μg of emetine hydrochloride and 30-10 μg of emetine hydrochloride;

[0056] (3) Preparation of the test solution Precisely draw 20ml of ipecac tincture, put it in a 25ml measuring bottle, add 60% m...

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Abstract

The invention relates to a HPLC (High Performance Liquid Chromatography) quantitative method for cephaeline hydrochloride and ipecine hydrochloride in an ipecacuanha medicinal material and a preparation of ipecacuanha medicinal material. The method is characterized by comprising the following steps: firstly, performing common isocratic elution according to PHLC method, and taking acetonitrile-carbinol-0.1% of phosphoric acid at a volume ratio of (8-9.5):(3-5):(86-88) as a flowing phase, wherein a detecting wavelength is 205nm; and simultaneously measuring the contents of the cephaeline hydrochloride and ipecine hydrochloride in the ipecacuanha medicinal material and a fluid extract, extract and tincture thereof so as to end the history of the measurement of total alkaloids of the ipecacuanha alkaloids in an acid base titration form according to the standard in multiple countries: after performing column chromatography separation for 4 times, respectively measuring the cephaeline hydrochloride and ipecine hydrochloride through delta A at 283nm and 350nm by adopting differential spectrophotometry. According to the method, only acidic aqueous carbinol or aqueous carbinol is used; after fine powder of the medicinal material is ultrasonically extracted or each preparation is diluted, a certain amount of subsequent filtrate is absorbed; and an alumina column is used for removing impurities so as to measure. The method is quick, convenient, accurate and capable of reappearing.

Description

technical field [0001] The invention relates to an HPLC quantitative method for ipecine hydrochloride and ipecine hydrochloride in ipecac medicinal materials and preparations thereof. Background technique [0002] Ipeca is the dry rhizome of Cephaelis ipecacuanha (Brot.) A.Rich. or Cephaelis acuminata Karsten. It is an expectorant and antitussive. It is a medicinal material imported from Brazil, Costa Rica or India, and it is recorded in the United States Pharmacopoeia (24 edition) and the European Pharmacopoeia (7.0). The United States Pharmacopoeia contains the quality standards of ipecac medicinal material, ipecac powder and ipecac syrup, and the content determination thereof is as follows: respectively measuring the contents of ipecac total alkaloids, ipecac and ipecac. After the total alkaloids were extracted with chloroform, the acid-base back titration method was used to determine the total alkaloid content. The content determination of emetine and emetine is extre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/88
Inventor 韩桂茹贾永鑫封淑华
Owner JING JING PHARMA
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