Method of detecting apovincamine acid and vincamine acid in vinpocetine simultaneously

A technology of apo-vinblastine and vinpocetine is applied in the field of analytical chemistry to achieve the effects of high peak symmetry, high system adaptability and high precision

Inactive Publication Date: 2019-11-15
武汉华龙生物制药有限公司
View PDF4 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methods reported in the above two literatures are not suitable for the simultaneous detection of apovincine and vinblastine in vinpocetine.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method of detecting apovincamine acid and vincamine acid in vinpocetine simultaneously
  • Method of detecting apovincamine acid and vincamine acid in vinpocetine simultaneously
  • Method of detecting apovincamine acid and vincamine acid in vinpocetine simultaneously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Instruments and reagents

[0045] (1) LC-20AD high performance liquid chromatograph (Japan Shimadzu company), including LC-20AD pump, SPD-M20A diode array detector (190nm~800nm), SIL-20A automatic sampler, Labsolution workstation; E2695 high performance liquid chromatograph (U.S. Waters company), including 2998 diode array detector (190nm ~ 800nm), Empower3 workstation; AUW 220D double range analytical balance (sensitivity 0.1mg / 0.01mg, Japan Shimadzu company); SHH-100GD-2 drug strong light irradiation test chamber (Chongqing Yongsheng Experimental Instrument Factory); GXZ-9240 MBE blast drying oven (Shanghai Boxun Industrial Co., Ltd. Medical Equipment Factory)

[0046] (2) Reagents: Except for methanol, which is chromatographic grade, other reagents are analytically pure.

[0047] (3) Reference substance: Vinpocetine reference substance (CAS: 42971-09-5), batch number: 100947-201203, provided by China National Institutes for Food and Drug Control. Apvincine refer...

experiment example 1

[0078] Experimental Example 1 System Suitability Test and Interference Test

[0079] 1. Take 10 μl of the system suitability solution and inject it into the liquid chromatograph, and record the chromatogram. The system suitability solution: take an appropriate amount of vinpocetine, vinblastine and apovincine acid reference substance, add mobile phase A- Methanol (60:40) was dissolved and diluted to make a mixed solution containing about 1 μg of vinpocetine, 0.5 μg each of vincine and apovincine per 1 ml, as a system suitability solution.

[0080] Table 4 System Suitability Results

[0081] Compound name concentration retention time (min) Separation Vinpocetine 1μg / ml 39.146 43.9 vinblastine 0.5μg / ml 7.179 / Apovincine 0.5μg / ml 8.690 4.2

[0082] The result is as figure 1 As shown, the order of the peaks is vinblastine, apovincine, and vinpocetine. The main peak retention time of vinpocetine is 39.146 minutes, and the peak retent...

experiment example 2

[0085] Experimental example 2 Forced degradation test

[0086] In order to further investigate the impact of impurities or degradation products that may exist in the sample on the determination of vincine and apovincine, this method carried out a forced degradation test. Through strong light irradiation, high temperature, acid-base hydrolysis, oxidation and other methods, the destruction of vinpocetine and vinpocetine injection is accelerated, and the separation of degradation products and unknown impurities of samples from vinblastine and apovincine acid is investigated. , to evaluate the validity and applicability of the method.

[0087] 1. Forced degradation test of vinpocetine raw material

[0088] Under the conditions of light and high temperature destruction, vinpocetine was basically not degraded, and no vincine and apovincine were detected in the suspension and powder destruction samples, and the stability was good. Under the conditions of oxidation, alkali, and acid...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
concentrationaaaaaaaaaa
separationaaaaaaaaaa
recovery rateaaaaaaaaaa
Login to view more

Abstract

The invention provides a method of detecting apovincamine acid and vincamine acid in vinpocetine simultaneously. The method comprises steps of (1) preparing a test solution by using a vinpocetine rawmaterial or vinpocetine injection; (2) diluting the test solution by 1000 times to be used as a control solution; (3) performing chromatographic separation on the test solution and the control solution by using high-performance liquid chromatography, and recording a chromatograph, wherein chromatographic conditions are as follows: detection wavelength is 262nm-266nm, column temperature is 25DEG C-35DEG C, a mobile phase A is a phosphate buffer solution, a mobile phase B is methanol, and eluting flow rate is 0.8-1.5ml/min; and (4) calculating contents of apovincamine acid and vincamine acid inthe test solution according to a self-control method of a principle component with a calibration factor. Peaks of the vincamine acid and apovincamine acid and the peak of vinpocetine can be well separated. The method can highly adapt to a system, and has low detection limit and high precision.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for simultaneously detecting apovincine and vinblastine in vinpocetine. Background technique [0002] Impurities in drugs refer to substances in drugs that have no therapeutic effect or affect the stability and curative effect of drugs, and are even harmful to human health. In the research, production, storage and clinical application of drugs, it is necessary to maintain the purity of drugs and reduce the impurities of drugs, so as to ensure the effectiveness and safety of drugs. [0003] Vinpocetine is a derivative of alkaloid extracted from Vinca minor in Apocynaceae, and its active ingredient is apovincine ethyl ester. Vinpocetine has multiple effects and can improve brain metabolism, blood flow and hemorheological properties. The vinpocetine raw materials used in this product have many impurities, which mainly come from the reaction raw materials, syn...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/36G01N30/74G01N30/8679G01N2030/027
Inventor 丁冠军刘薇汪秋兰董辉黄楚华吴芬
Owner 武汉华龙生物制药有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap