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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
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  • 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-phase liquid chromatography is poor, so it is necessary to develop a method for effectively detecting the impurities of clevidipine butyrate

Method used

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  • 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

Embodiment 1

[0031] Dissolving sample solvent and concentration selection

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

[0033] When the mobile phase is used as the solvent of the sample, the mobile phase is formulated 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 0.2 mg / ml is used, and when 1.0 mg / ml is used, the concentration of the mobile phase is too large to be conducive to the separation of the sample, so the final choice is 0.5 mg / ml as the concentration of the test solution.

Embodiment 2

[0035] Adopt American Agilent 1260 high performance liquid chromatograph, autosampler; Welchrom C18 column; Mobile phase volume ratio is acetonitrile: ethanol: water=16:40:44; Injection volume is 20 μ l; Detection wavelength is 240nm; Flow rate is 1.0 ml / min; column temperature is 35°C.

[0036] Experimental steps:

[0037] Get clevidipine butyrate and its impurity Ⅰ, Ⅲ, Ⅳ, Ⅴ amount, dissolve and dilute with mobile phase to make every 1ml contain clevidipine butyrate 0.50mg, impurity 0.5μg solution, shake well, as the test sample solution. Inject and measure according to the above conditions, record the chromatogram, the results are shown in figure 1 . figure 1 It shows that the separation between clevidipine butyrate and its impurities and between impurities and impurities meets the requirements.

Embodiment 3

[0039] Adopt American Agilent 1260 high performance liquid chromatograph, autosampler; WelchromC18 column (4.6 * 250mm, 5 μ m); Mobile phase is methanol: ethanol: water = 15: 45: 40; Injection volume is 20 μ l; Detection wavelength is 240nm ; The flow rate is 1.0ml / min; The column temperature is 40°C.

[0040] Experimental steps:

[0041] Get clevidipine butyrate and its impurity Ⅰ, Ⅲ, Ⅳ, Ⅴ amount, dissolve and dilute with mobile phase to make every 1ml contain clevidipine butyrate 0.50mg, impurity 0.5μg solution, shake well, as the test sample solution. Inject and measure according to the above conditions, record the chromatogram, the results are shown in figure 2 . figure 2 It shows that the separation between clevidipine butyrate and its impurities and between impurities and impurities meets the requirements

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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

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Application Information

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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
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