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Analysis and detection method for 7-fluoro-4-hydroxyquinazoline

A technology of hydroxyquinazoline and detection method, applied in the field of high performance liquid chromatography analysis, can solve the problems affecting the quality of final product afatinib and the like

Active Publication Date: 2017-12-19
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The analysis and detection method of this intermediate has not been recorded in the literature, but the analysis and detection of this intermediate has an important effect on reaction control and yield improvement, and also directly affects the quality of the final product afatinib, so a stable method is established. Effective analysis and detection methods are necessary for quality control of this intermediate

Method used

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  • Analysis and detection method for 7-fluoro-4-hydroxyquinazoline
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  • Analysis and detection method for 7-fluoro-4-hydroxyquinazoline

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Experimental program
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Effect test

Embodiment 1

[0028] Instrument and conditions: Agilent 1260 liquid chromatography system, chromatographic column: welch Ultimate XB-C18 (4.6 × 250mm, 3μm), detection wavelength 247nm, column temperature 30 ℃, flow rate 1.0ml / min, with 0.1% phosphoric acid aqueous solution (volume ratio ) is mobile phase A, with acetonitrile as mobile phase B, in volume ratio, the setting of gradient elution is:

[0029]

[0030] Experimental procedure: Dissolve 7-fluoro-4-hydroxyquinazoline with 0.1% phosphoric acid aqueous solution and acetonitrile at a volume ratio of 90:10 and quantitatively dilute to prepare 0.2 mg of 7-fluoro-4-hydroxyquinazoline per 1 ml Solution, as the test solution, accurately measure 10 μ l of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, and the results are shown in the attached figure 1 .

[0031] attached figure 1 Show that under this chro...

Embodiment 2

[0033] Instrument and conditions: Agilent 1260 liquid chromatography system, chromatographic column: welch Ultimate XB-C18 (4.6 × 250mm, 3μm), detection wavelength 247nm, column temperature 30 ℃, flow rate 0.7ml / min, with 0.05% phosphoric acid aqueous solution (volume ratio ) is mobile phase A, with acetonitrile as mobile phase B, in volume ratio, the setting of gradient elution is:

[0034]

[0035]

[0036] Experimental procedure: Dissolve 7-fluoro-4-hydroxyquinazoline with 0.1% phosphoric acid aqueous solution and acetonitrile at a volume ratio of 90:10 and quantitatively dilute to prepare 0.2 mg of 7-fluoro-4-hydroxyquinazoline per 1 ml Solution, as the test solution, accurately measure 10 μ l of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, and the results are shown in the attached figure 2 .

[0037] attached figure 2 Show that ...

Embodiment 3

[0039] Instrument and conditions: Agilent 1260 liquid chromatography system, chromatographic column: welch Ultimate XB-C18 (4.6 × 250mm, 3μm), detection wavelength 247nm, column temperature 30 ℃, flow rate 1.1ml / min, with 0.15% phosphoric acid aqueous solution (volume ratio ) is mobile phase A, with acetonitrile as mobile phase B, in volume ratio, the setting of gradient elution is:

[0040]

[0041] Experimental procedure: Dissolve 7-fluoro-4-hydroxyquinazoline with 0.1% phosphoric acid aqueous solution and acetonitrile at a volume ratio of 90:10 and quantitatively dilute to prepare 0.2 mg of 7-fluoro-4-hydroxyquinazoline per 1 ml Solution, as the test solution, accurately measure 10 μ l of the test solution and inject it into the liquid chromatograph, carry out high-performance liquid chromatography analysis according to the above conditions, record the chromatogram, and the results are shown in the attached image 3 .

[0042] attached image 3 Show that under this chr...

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Abstract

The invention relates an analysis and detection method for 7-fluoro-4-hydroxyquinazoline. The analysis and detection method is used for quality control of 7-fluoro-4-hydroxyquinazoline and carries out high-performance liquid chromatographic analysis and detection under the conditions that a chromatographic column (C18, 4.6*250 mm, 3[mu]m) is packed with octadecylsilane bonded silica gel; an aqueous phosphoric acid solution with a concentration of 0.05-0.15% and acetonitrile are used as mobile phases; gradientelution is carried out; detection wavelength is 247 nm; and column temperature is 25 to 35 DEG C. The analysis and detection method can effectively separate 7-fluoro-4-hydroxyquinazoline from impurities and has the advantages of high resolution and sensitivity, good repeatability and durability, short analysis time, simple operation and 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 for 7-fluoro-4-hydroxyquinazoline. Background technique [0002] Afatinib is an aniline quinazoline compound, an irreversible EGFR-HER2 dual tyrosine kinase receptor inhibitor, which can irreversibly bind to EGFR-HER2 tyrosine kinase and inhibit its tyrosine kinase activity, thereby blocking the tumor cell signal transduction dominated by EGFR-HER2, inhibiting the metastasis and proliferation of tumor cells, and promoting the apoptosis of tumor cells. [0003] 7-fluoro-4-hydroxyquinazoline is one of the important intermediates for the synthesis of afatinib, and its chemical formula is C 8 h 5 FN 2 O, the structural formula is: [0004] [0005] The analysis and detection method of this intermediate has not been recorded in the literature, but the analysis and detection of this intermediate has an important effect o...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 张贵民王芳
Owner SHANDONG NEWTIME PHARMA
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