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Method for determining contents of impurity compounds I in nilotinib

A technology for nilotinib and compounds, which can be used in measurement devices, instruments, scientific instruments, etc., and can solve the problems of inability to provide trace analysis results, specificity, sensitivity, method precision and repeatability defects.

Inactive Publication Date: 2017-07-07
SHANGHAI AOBO PHARMTECH INC LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, only the method for determining the content of constant 3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)aniline in nilotinib adopts classical chromatography, and its specificity, Sensitivity, method precision, and repeatability are largely deficient and do not provide reliable trace analysis results

Method used

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  • Method for determining contents of impurity compounds I in nilotinib
  • Method for determining contents of impurity compounds I in nilotinib
  • Method for determining contents of impurity compounds I in nilotinib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instruments and Conditions:

[0037] High performance liquid chromatography mass spectrometry: Agilent 1260 infinity, MS detector.

[0038] Chromatographic column: Octadecylsilane bonded silica gel column

[0039] Mobile phase: A: 0.05%-0.2% formic acid or acetic acid or trifluoroacetic acid aqueous solution B: acetonitrile.

[0040] The isocratic is as follows: 0-8.0min, the proportion of the organic phase changes from 10% to 90%.

[0041] Column temperature: 35°C.

[0042] Flow rate: 1.0mL / min

[0043] Select positive ions: 242

[0044] Injection volume: 5ul.

[0045] Experimental steps:

[0046] 1) Preparation of mobile phase A: Precisely measure 1.0 mL of trifluoroacetic acid and dissolve in 1000 mL of water, and mix well.

[0047] 2) Diluent B: Acetonitrile

[0048] 3) Standard solution C: Accurately weigh about 28.5mg of compound I in a 100ml volumetric flask, add B to dissolve to volume, shake well, accurately measure 2.0ml and place it in another 100ml v...

Embodiment 2

[0050] Instruments and Conditions:

[0051] High performance liquid chromatography: Agilent 1260 infinity, MS detector.

[0052] Chromatographic column: Octadecylsilane bonded silica gel column

[0053] Mobile phase: A: 0.05%-0.2% formic acid or acetic acid or trifluoroacetic acid aqueous solution B: acetonitrile.

[0054] The isocratic is as follows: 0-8.0min, the proportion of the organic phase changes from 10% to 90%.

[0055] Column temperature: 35°C.

[0056] Flow rate: 1.0mL / min

[0057] Select positive ions: 242

[0058] Injection volume: 5ul.

[0059] Experimental steps:

[0060] 1) Preparation of mobile phase A: Precisely measure 1.0 mL of trifluoroacetic acid and dissolve in 1000 mL of water, and mix well.

[0061] 2) Diluent B: Acetonitrile

[0062] 3) Standard solution C: Accurately weigh about 28.5mg of compound I in a 100ml volumetric flask, add B to dissolve to volume, shake well, accurately measure 2.0ml and place it in another 100ml volumetric flask, a...

Embodiment 3

[0065] Instruments and Conditions:

[0066] High performance liquid chromatography: Agilent 1260 infinity, MS detector.

[0067] Chromatographic column: Octadecylsilane bonded silica gel column

[0068] Mobile phase: A: 0.05%-0.2% formic acid or acetic acid or trifluoroacetic acid aqueous solution B: acetonitrile.

[0069] The isocratic is as follows: 0-8.0min, the proportion of the organic phase changes from 10% to 90%.

[0070] Column temperature: 35°C.

[0071] Flow rate: 1.0mL / min

[0072] Select positive ions: 242

[0073] Injection volume: 5ul.

[0074] Experimental steps:

[0075] 1) Preparation of mobile phase A: Precisely measure 1.0 mL of trifluoroacetic acid and dissolve in 1000 mL of water, and mix well.

[0076] 2) Diluent B: Acetonitrile

[0077]3) Standard solution C: Accurately weigh about 28.5mg of compound I in a 100ml volumetric flask, add B to dissolve to volume, shake well, accurately measure 2.0ml and place it in another 100ml volumetric flask, ad...

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Abstract

The invention discloses a method for determining and analyzing the content of 3-(4-methyl-1H-imidazole-1-yl)-5-(trifluoromethyl) aniline in nilotinib. The content of the 3-(4-methyl-1H-imidazole-1-yl)-5-(trifluoromethyl) aniline in the nilotinib is directly measured by the aid of efficient liquid chromatography-mass spectrometers. Compared with the prior art, the method has the advantages of good specificity and repeatability, extremely high sensitivity, suitability for trace analysis and the like.

Description

technical field [0001] The present invention relates to direct determination of 3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)aniline (hereinafter referred to as nilotinib) with high performance liquid chromatography-mass spectrometry Compound I) content. The method can better control the content of trace compound I in raw materials and preparations, and can provide protection for patients' health and safety in drug use, and belongs to the technical field of medicine. [0002] technical background [0003] Nilotinib, chemical name Nilotinib. [0004] It is a drug for the treatment of adult patients with Philadelphia chromosome positive chronic myelogenous leukemia (Ph+CML) in chronic phase or accelerated phase who are resistant or intolerant to previous treatment. The structure of nilotinib is as follows: [0005] [0006] Nilotinib contains compound I, a reaction residue, with the following structure: [0007] [0008] Accurate and quantitative determination of ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884G01N2030/8872
Inventor 邱学艳顾虹安建国胡素招
Owner SHANGHAI AOBO PHARMTECH INC LTD
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