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Method for detecting clevidipine butyrate and related substances in preparations of clevidipine butyrate

A clevidipine butyrate and detection method technology, applied in the field of medicine, can solve problems such as interference, inability to separate, and no uniform drug standards for drugs

Active Publication Date: 2015-05-06
WUHAN CONFORM PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It has been verified that under the conditions of this method, the separation degree of degradation H207 / 59 of clevidipine butyrate and impurity G is 1.06, which cannot be separated. / 78 cannot achieve sufficient separation, and the resolution is only 1.31
[0014] At present, there is no literature report on the analytical method of clevidipine butyrate in China, and there is no uniform drug standard for this drug. Therefore, in order to better control the quality of clevidipine butyrate products, it is necessary to establish a set of simple, reliable and stable An effective method to detect the related substances of this product, and solve the interference of various known or unknown impurities introduced by the synthesis process or degradation and preparation process on the determination of product purity

Method used

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  • Method for detecting clevidipine butyrate and related substances in preparations of clevidipine butyrate
  • Method for detecting clevidipine butyrate and related substances in preparations of clevidipine butyrate
  • Method for detecting clevidipine butyrate and related substances in preparations of clevidipine butyrate

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Experimental program
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Effect test

Embodiment 1

[0049] Embodiment 1 acetonitrile: methanol: phosphate buffer solution (pH=3.0)=40:20:40 (volume ratio) is the test that the mobile phase cannot completely separate the mixed solution of known impurities

[0050] 1. Instruments: Agilent 1260 high performance liquid chromatography, electronic analytical balance, pH meter.

[0051] 2. Determination method: Accurately weigh an appropriate amount of reference substances of clevidipine butyrate, impurity G, impurity F and reference substances of H324 / 78, H168 / 79, H207 / 59, H152 / 81 and H152 / 66, add methanol to dissolve And be diluted into the known impurity mixed solution that contains clevidipine butyrate 1mg and each impurity about 1 μ g in every 1ml as need testing solution. Chromatographic column Waters sunfire C18 150×4.6mm, 3.5μm; mobile phase is acetonitrile: methanol: phosphate buffer solution = 40:20:40, phosphate buffer solution consists of 15ml 1mol / L phosphoric acid and 100ml 1mol / L sodium dihydrogen phosphate Mix, add wa...

Embodiment 2

[0052] Embodiment 2 acetonitrile: methanol: phosphate buffer solution (pH=3.0)=40:20:40 (volume ratio) is the test that the mobile phase cannot completely separate the mixed solution of known impurities

[0053] 1. Instruments: Agilent 1260 high performance liquid chromatography, electronic analytical balance, pH meter.

[0054] 2. Determination method (1): Accurately weigh an appropriate amount of reference substances of impurities A~I and reference substances of H324 / 78, H168 / 79, H207 / 59, H152 / 81 and H152 / 66, add methanol to dissolve and dilute to each A mixed solution of known impurities containing about 20 μg of each impurity in 1 ml was used as the test solution. Chromatographic column Hypersil BDS C18150×4.6mm, 3μm; mobile phase is acetonitrile:methanol:phosphate buffer solution=40:20:40, phosphate buffer solution consists of 15ml 1mol / L phosphoric acid and 100ml 1mol / L phosphoric acid di Mix sodium hydrogen, add water to dilute to 2000ml, and adjust pH to 3.0 with phos...

Embodiment 3

[0055] Example 3 Acetonitrile-0.01mol / L ammonium dihydrogen phosphate buffer solution as the mobile phase and gradient elution with different ratios can not completely separate the test of the mixed solution of known impurities

[0056] 1. Instruments: Agilent 1260 high performance liquid chromatography, electronic analytical balance, pH meter.

[0057] 2. Determination method (1): Accurately weigh the reference substances of clevidipine butyrate, impurity G, impurity F and the reference substances of H324 / 78, H168 / 79, H207 / 59, H152 / 81 and H152 / 66. Add methanol to dissolve and dilute to a mixed solution of known impurities containing 1 mg clevidipine butyrate and about 1 μg of each impurity in every 1 ml as the test solution. Chromatographic column Waters sunfire C18 150×4.6mm, 3.5μm; mobile phase system, A is acetonitrile, B is 0.01mol / L ammonium dihydrogen phosphate buffered saline buffer solution, 0.01mol / L ammonium dihydrogen phosphate buffer solution is prepared by 1.15g ...

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Abstract

The invention discloses a method for detecting clevidipine butyrate and related substances in preparations of the clevidipine butyrate. The method is characterized in that gradient elution is carried out by virtue of a C18 chromatographic column by taking methanol-acetonitrile-phosphate buffer salt solution as a mobile phase according to a reversed-phase high-performance liquid chromatography and an ultraviolet detector is used. By means of the method, effective separation of the clevidipine butyrate from all known impurities can be realized; interference of various impurities generated in the synthesis and preparation production processes to the purity of products can be avoided; the quantity of the clevidipine butyrate or preparations can be controlled comprehensively and effectively; the method is simple to operate and high in specificity and sensitivity and is capable of well detecting the clevidipine butyrate and related substances in the preparations; and an effective and reliable analysis method is provided for quality control of research, development and production processes.

Description

technical field [0001] The invention belongs to the technical field of medicines, in particular to a method for detecting related substances in clevidipine butyrate and its preparations. Background technique [0002] The drug name of clevidipine butyrate described in the present invention is: [0003] Generic Name: Clevidipine Butyrate [0004] Chemical name: Methyl(1-butyryloxy)methyl 4-(2,3-dichlorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarboxylate 4-(2,3-dichlorophenyl)-1,4-dihydro-2,6-dimethyl-3,5-Pyridinedicarboxylic acid methyl(1-oxobutoxy)methyl ester [0005] English name: Clevidipine butyrate [0006] Chemical Structure: [0007] [0008] Molecular formula: C 21 h 23 Cl 2 NO 6 [0009] Molecular weight: 456.32 [0010] Clevidipine butyrate is a third-generation novel short-acting dihydropyridine calcium channel antagonist developed by AstraZeneca. Clevidipine butyrate emulsion for intravenous injection was first launched in the United States in...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N33/15
Inventor 周小顺牟东升饶敦艳李进贺容丽李彤彤
Owner WUHAN CONFORM PHARMA CO LTD
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