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A kind of analysis and detection method of dasatinib intermediate

A technology for dasatinib and intermediates, applied in the field of analysis and detection of dasatinib intermediates, can solve problems such as unsuitable for popularization, high price of chromatographic columns, long analysis time, etc., and achieve stable and reliable results and peak shape The effect of good symmetry and short analysis time

Active Publication Date: 2018-07-31
SHANDONG NEWTIME PHARMA
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0005] The analysis and detection of dasatinib intermediates plays an important role in reaction control and yield improvement, and also directly affects the quality of the final product. The literature of Alban J.Allentoff et al. (Synthesis of 14 C-labeled and 13 C-, 15 N-labeled dasatinib and its piperazine N-dealkyl metabolite, J.LabelCompd.Radiopharm2008, 51: 41–47) discloses an HPLC analysis method for this intermediate, but this method is cumbersome, takes a long time to analyze, and uses Chromatographic columns are relatively expensive, and are generally used in R&D and production with low practicability, so they are not suitable for popularization. Therefore, it is necessary to establish a low-cost, stable and effective analysis and detection method that uses ordinary chromatographic columns and liquid phase systems and is simple to operate. It is very necessary to analyze and detect dasatinib intermediates

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  • A kind of analysis and detection method of dasatinib intermediate
  • A kind of analysis and detection method of dasatinib intermediate
  • A kind of analysis and detection method of dasatinib intermediate

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Embodiment 1

[0032] Instruments and conditions: Agilent1100 liquid chromatography system, DAD detector, chromatographic column: Boston BoschromODS C18 (4.6×250mm, 5μm), detection wavelength 320nm, column temperature 25°C, flow rate 1.0mL / min, mobile phase: 0.05mol / L Sodium acetate solution: acetonitrile=55:45, the volume of trifluoroacetic acid is 0.2% of the volume sum of the former two.

[0033] Experimental procedure: Dissolve the intermediate of dasatinib with the mobile phase and quantitatively dilute it to make a solution containing 0.2 mg of the intermediate of dasatinib per 1 mL, as the test solution, accurately measure 10 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 1 .

[0034] attached figure 1 It shows that under the chromatographic conditions, the peak of Dasatinib intermediate and the impurity peak can be compl...

Embodiment 2

[0036] Instruments and conditions: Agilent1100 liquid chromatography system, DAD detector, chromatographic column: Boston BoschromODS C18 (4.6×250mm, 5μm), detection wavelength 320nm, column temperature 25°C, flow rate 0.5mL / min, mobile phase: 0.01mol / L Sodium acetate solution: acetonitrile = 65:35, the volume of trifluoroacetic acid is 0.2% of the volume sum of the former two.

[0037] Experimental procedure: Dissolve the intermediate of dasatinib with the mobile phase and quantitatively dilute it to make a solution containing 0.2 mg of the intermediate of dasatinib per 1 mL, as the test solution, accurately measure 10 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached figure 2 .

[0038] attached figure 2 It shows that under the chromatographic conditions, the peak of Dasatinib intermediate and the impurity peak can be c...

Embodiment 3

[0040] Instruments and conditions: Agilent1100 liquid chromatography system, DAD detector, chromatographic column: Boston BoschromODS C18 (4.6×250mm, 5μm), detection wavelength 320nm, column temperature 25°C, flow rate 1.2mL / min, mobile phase: 0.03mol / L Sodium acetate solution: acetonitrile = 45:55, the volume of trifluoroacetic acid is 0.2% of the volume sum of the former two.

[0041] Experimental procedure: Dissolve the intermediate of dasatinib with the mobile phase and quantitatively dilute it to make a solution containing 0.2 mg of the intermediate of dasatinib per 1 mL, as the test solution, accurately measure 10 μL of the test solution for injection Phase chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram, the result sees attached image 3 .

[0042] attached image 3 It shows that under the chromatographic conditions, the peak of Dasatinib intermediate and the impurity peak can be com...

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Abstract

The invention discloses an analysis and detection method of a dasatinib intermediate, which is used for the quality control of the dasatinib intermediate, and uses octadecylsilane bonded silica gel as a chromatographic column (C18, 4.6×250mm , 5 μm), using the mixed system of buffered saline, acetonitrile and trifluoroacetic acid as the mobile phase, the detection wavelength is 320nm, and the column temperature is 20-30°C, for high-performance liquid chromatography analysis and detection. The analysis and detection method of the present invention selects common chromatographic columns and liquid chromatography systems, is cheap, and has high practicability, and can effectively separate dasatinib intermediates and impurities thereof, and the method has short analysis time, high sensitivity, Good linear relationship, simple operation, good repeatability and durability, stable and reliable results.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography analysis method, in particular to an analysis and detection method of a dasatinib intermediate. Background technique [0002] Dasatinib is an oral tyrosine kinase inhibitor approved by the FDA in 2006 for the treatment of leukemia caused by BCR-ABL kinase mutation, its efficacy is better than that of imatinib, and no drug resistance has been found . [0003] N-(2-chloro-6-methylphenyl)-2-[(6-chloro-2-methyl-4-pyrimidinyl)amino]-5-thiazole carboxamide is an important intermediate of dasatinib , whose chemical formula is C 16 h 13 Cl 2 N 5 OS, the structural formula is: [0004] [0005] The analysis and detection of dasatinib intermediates plays an important role in reaction control and yield improvement, and also directly affects the quality of the final product. The literature of Alban J.Allentoff et al. (Synthesis of 14 C-labeled and 13 C-, 15 N-labeled dasatinib and its pi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 赵志全
Owner SHANDONG NEWTIME PHARMA