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A method for separating conitinib and related substances by liquid chromatography

A technology for conitinib and related substances, which is applied in the field of drug analysis and can solve problems such as adverse drug reactions

Active Publication Date: 2019-01-01
BEIJING KONRUNS PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Conitinib and its preparations are a new class of anti-tumor chemical drugs. At present, there is no national standard. Through literature search, there is no report on the drug analysis method for the detection of conitinib-related substances, and the relevant substances are drug quality. An important indicator of control, related to possible adverse reactions of drugs

Method used

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  • A method for separating conitinib and related substances by liquid chromatography
  • A method for separating conitinib and related substances by liquid chromatography
  • A method for separating conitinib and related substances by liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Embodiment 1: Determination of detection wavelength

[0083] 1) Experimental steps:

[0084] Using methanol as a solvent, a total of 8 solutions containing conitinib and its 7 impurities (impurity I-impurity VII) were prepared respectively, and the concentration of each solution was about 10 μg / ml.

[0085] Using methanol solvent as a blank, the solution of conitinib and various related substances was scanned by ultraviolet detection, and the scanning wavelength range was 200-400nm.

[0086] 2) Experimental results: Conitinib and related substances have strong absorption in the wavelength range of 220-270nm, and each sample has strong absorption at 250nm wavelength.

[0087] Therefore, the present invention selects 250nm as the detection wavelength.

[0088] In addition, the detection wavelength has also been verified by destroying experimental samples.

Embodiment 2

[0089] Embodiment 2: the screening of mobile phase

[0090] 1) Chromatographic conditions

[0091] Chromatographic column: the chromatographic column filler is octylsilane bonded silica gel with a particle size of 3.5 μm, and the chromatographic column specification is 150mm×4.6mm, purchased from Waters;

[0092] Mobile phase flow rate: 1.0ml / min;

[0093] Injection volume: 5μl;

[0094] Column temperature: 30°C;

[0095] Detection wavelength: 250nm.

[0096] 2) Preparation of the test solution: take 30 mg of conitinib and 3 mg of its related substances respectively, mix and place in a 100 ml volumetric flask, add solvent (0.05% trifluoroacetic acid aqueous solution and 0.05% trifluoroacetic acid acetonitrile solution) According to the mixed solution prepared with a volume ratio of 30:70), dissolve and dilute to the mark, shake well, and the test solution is ready.

[0097] 3) Screening of the aqueous phase

[0098] Mobile phase A is water, mobile phase B is acetonitrile...

Embodiment 3

[0117] Embodiment 3: determination of limit of detection and limit of quantitation

[0118] 1) Chromatographic conditions

[0119] Chromatographic column: the chromatographic column filler is octylsilane bonded silica gel with a particle size of 3.5 μm, and the chromatographic column specification is 150mm×4.6mm, purchased from Waters;

[0120] Mobile phase: Mobile phase A is a 0.05% trifluoroacetic acid aqueous solution, and mobile phase B is a 0.05% trifluoroacetic acetonitrile solution, and the elution gradient is eluted as shown in Table 1 in Example 1:

[0121] Mobile phase flow rate: 1.0ml / min;

[0122] Injection volume: 5μl;

[0123] Column temperature: 30°C;

[0124]The detection wavelength is 250nm.

[0125] 2) Preparation of sample solution: Weigh 30 mg of the standard product conitinib and related substances, put them in 100 ml measuring bottles respectively, mix them with solvent (mobile phase A and mobile phase B prepared according to the volume ratio of 70:30...

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Abstract

The invention relates to a method for separating conitinib and related substances by liquid chromatography, and the method is high performance liquid chromatography. The method provided by the present invention can complete the effective separation of conitinib and its seven related substances, can comprehensively detect and control the impurities of related substances that may exist in conitinib, and can also be used for conitinib and its seven related substances. Accurate quantification of its related substances. The method is stable, reliable, and highly sensitive, and can be used for the research of conitinib bulk drug and its preparations and the quality control in the production process.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for separating conitinib and its related substances. Background technique [0002] Kanitinib is a new class of chemical anti-tumor drug independently developed by Beijing Kangchen Pharmaceutical Co., Ltd. It mainly acts on the hepatocyte growth factor receptor (hepatocyte growth factor receptor, or mesenchymal–epithelial transition factor, c- MET) and vascular endothelial growth factor 2 (vascular endothelial growth factor receptor, VEGFR2 or KDR) novel multi-target receptor tyrosine kinase inhibitors. It is suitable for advanced gastroesophageal junction adenocarcinoma with c-Met gene amplification and advanced castration-resistant prostate cancer with bone metastases. [0003] The chemical name of conitinib is N1-[4-[[7-[[1-(diethoxyphosphorylmethyl)-4-piperidinyl]methoxy]-6-methoxy-4 -quinolyl]oxy]-3-fluorophenyl]-N1'-(4-fluorophenyl)cyclopropane-1,1-dicarboxa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 陈东郑亚彬曹相林王锡娟其他发明人请求不公开姓名
Owner BEIJING KONRUNS PHARM CO LTD