Clevidipine butyrate related substance detection method

A clevidipine butyrate and detection method technology, which is applied in the field of drug analysis, can solve problems such as poor separation effect, and achieve the effects of simple method, high sensitivity and specificity, and strong operability

Inactive Publication Date: 2017-11-21
天津康鸿医药科技发展有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Because the difference between clevidipine butyrate and its impurities is small, the method separation effect of general reversed-p

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
  • Clevidipine butyrate related substance detection method
  • Clevidipine butyrate related substance detection method
  • Clevidipine butyrate related substance detection method

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0030] Example 1

[0031] Choice of solvent and concentration for dissolving sample

[0032] For the choice of solvent for dissolving the sample, dissolve the sample with acetonitrile, methanol, and mobile phase, and they can all be dissolved. To reduce the appearance of solvent peaks, use mobile phase to dissolve the sample.

[0033] When using the mobile phase as the solvent of the sample, the mobile phase is prepared into three concentrations of 0.2mg / ml, 0.5mg / ml and 1.0mg / ml respectively. Although these three concentrations can achieve the separation of impurities, the detection response value is too small when 0.2mg / ml is used, and when 1.0mg / ml is used, the mobile phase concentration is too large and is not conducive to the separation of samples, so the final choice is 0.5 mg / ml is used as the concentration of the test solution.

Example Embodiment

[0034] Example 2

[0035] Use Agilent 1260 high-performance liquid chromatograph, autosampler; Welchrom C18 column; mobile phase volume ratio: acetonitrile: ethanol: water = 16:40:44; injection volume is 20μl; detection wavelength is 240nm; flow rate is 1.0 ml / min; the column temperature is 35°C.

[0036] Experimental steps:

[0037] Take appropriate amount of clevidipine butyrate and its impurities Ⅰ, Ⅲ, Ⅳ, and Ⅴ, dissolve and dilute with mobile phase to make a solution containing 0.50mg of clevidipine butyrate and 0.5μg of impurities per 1ml, shake it up and use it as the test product Solution. Inject the sample according to the above conditions, record the chromatogram, see the result figure 1 . figure 1 It shows that the separation degree between clevidipine butyrate and its impurities and between impurities and impurities meets the requirements.

Example Embodiment

[0038] Example 3

[0039] Use Agilent 1260 high performance liquid chromatograph, autosampler; Welchrom C18 column (4.6×250mm, 5μm); mobile phase: methanol: ethanol: water = 15:45:40; sample volume is 20μl; detection wavelength is 240nm ; The flow rate is 1.0ml / min; the column temperature is 40°C.

[0040] Experimental steps:

[0041] Take appropriate amount of clevidipine butyrate and its impurities Ⅰ, Ⅲ, Ⅳ, and Ⅴ, dissolve and dilute with mobile phase to make a solution containing 0.50mg of clevidipine butyrate and 0.5μg of impurities per 1ml, shake it up and use it as the test product Solution. Inject the sample according to the above conditions, record the chromatogram, see the result figure 2 . figure 2 Shows that the separation between clevidipine butyrate and its impurities and between impurities and impurities meet the requirements

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

No PUM Login to view more

Abstract

The invention provides a kind of detection method of clevidipine butyrate, the method adopts reversed-phase liquid chromatography, and the best chromatographic conditions are as follows: the chromatographic column is a Welchrom C18 chromatographic column; the mobile phase consists of methanol: ethanol: water=15~ 20:40~45:37~42 or acetonitrile:ethanol:water=16:40:44; the flow rate of the mobile phase is 1.0ml/min; the detection wavelength is 240nm; the column temperature is 40°C; the detector is an ultraviolet detector or a diode array detector. The detection method provided by the invention has high sensitivity and specificity, is simple and convenient to operate, and the degree of separation meets the requirements, and can quickly and accurately detect the content of various impurities in clevidipine butyrate, and can be used for the detection of clevidipine butyrate. Quality control is very important for the synthesis of antihypertensive drug clevidipine butyrate.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting related substances of clevidipine butyrate. Background technique [0002] The chemical name of Clevidipine butyrate is 4-(2',3'-dichlorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarboxylate Acid (butyryloxymethyl) (methyl) ester, the appearance is white crystalline powder, the molecular formula is C 21 h 23 Cl 2 NO 6 , with a molecular weight of 456.32 and a CAS accession number of 167221-71-8. The chemical structural formula of clevidipine butyrate is as follows: [0003] [0004] Clevidipine butyrate is an injectable antihypertensive drug used to treat acute hypertension, and its effect can last for 72 hours. Unlike existing high blood pressure drugs that are metabolized by the kidney or liver, clevidipine butyrate is metabolized in the blood and will not accumulate in the body, which is especially suitable for patients with advanced o...

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
IPC IPC(8): G01N30/89G01N30/06
CPCG01N30/89G01N30/06G01N2030/027G01N2030/062
Inventor 李银峰孙歆慧靳朝东邹美香陈晓雨刘钫
Owner 天津康鸿医药科技发展有限公司
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