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A method for simultaneous determination of gefitinib and related substances

A related substance, gefitinib technology, applied in the field of drug analysis, to achieve the effect of improving work efficiency, good linear relationship between peak area and concentration, and high sensitivity

Active Publication Date: 2018-11-20
NANJING YOKO PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to different impurities, this method is not suitable for the detection of related substances of gefitinib in our process

Method used

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  • A method for simultaneous determination of gefitinib and related substances
  • A method for simultaneous determination of gefitinib and related substances
  • A method for simultaneous determination of gefitinib and related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Embodiment 1 Chromatography condition selection

[0076] 1. Determination of detection wavelength

[0077] Preparation of diluent: measure 500mL of 0.2% trifluoroacetic acid solution, 500mL of methanol, stir and mix, the solution obtained is also a blank solution, measure with a UV spectrophotometer and gefitinib reference substance and its related substances at 200 The absorption wavelength in the ~400nm wavelength range, it was found that the gefitinib reference substance has large absorption at 218nm, 250nm and 340nm wavelength, but impurity II and impurity VII have large absorption at 250nm ~ 260nm, comprehensive consideration determines that the wavelength is 250nm.

[0078] 2. Mobile phase solvent selection

[0079] In the prior art, the mobile phase system is acetonitrile and ammonium acetate buffer solution, and the separation effect of gefitinib and impurities is poor. The present invention replaces mobile phase system, selects the mixed solution of acetonit...

Embodiment 2

[0098] Embodiment 2 System suitability experiment

[0099] Chromatographic conditions: Shimadzu LC-20A or Diane U3000 high-performance liquid chromatography system and workstation; automatic sample injection; Inert Sustain C 18 (100mm×3mm, 3μm) is the separation column; UV detection wavelength: 250nm; mobile phase A: 0.5% triethylamine solution / acetonitrile / methanol volume ratio is 90:5:5, mobile phase B: 0.5% triethylamine solution The volume ratio of / acetonitrile / methanol is 10:85:5, the column temperature is 50°C, the injection volume is 5 μL, and the flow rate is 0.5mL / min;

[0100] gradient program

[0101] time (min)

[0102] Get gefitinib impurity I, impurity II, impurity III, impurity IV, impurity V, impurity VI, impurity VII and impurity VIII reference substance with diluent (0.2% trifluoroacetic acid / methanol, volume ratio is 1:1) respectively Dissolve and quantitatively dilute to make a solution containing 10 μg per 1 mL, as the positioning solution for...

Embodiment 3

[0113] Example 3 Forced degradation experiment

[0114] The forced degradation experiment is to accelerate the destruction of gefitinib samples by means of strong light irradiation, high temperature, acid-base hydrolysis and oxidation under high intensity conditions. The separation of impurities, whether the material is balanced, and the effectiveness and applicability of the analytical method are evaluated.

[0115] Undamaged experiment: Take about 10 mg of gefitinib raw material, weigh it accurately, put it in a 10 mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, filter, and take the subsequent filtrate.

[0116] Acid destruction test: Take about 10 mg of gefitinib raw material, weigh it accurately, put it in a 10 mL measuring bottle, add 1 mL of 1 mol / L hydrochloric acid solution, heat in a water bath at 60 °C for 4 hours, add an equivalent amount of 1 mol / L sodium hydroxide solution And, add diluent to dilute to the mark, shake well, filter...

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Abstract

The invention provides an analysis and detection method for simultaneously measuring gefitinib and relevant substances thereof. By means of a high performance liquid chromatographic instrument, Inert Sustain C18 is used as a chromatographic column; for a flowing phase A: the volume ratio of 0.5% triethylamine solution to acetonitrile to methyl alcohol is 90 to 5 to 5; for a flowing phase B: the volume ratio of 0.5% triethylamine solution to acetonitrile to methyl alcohol is 10 to 85 to 5; during gradient elution, the detection wavelength is 240 to 260 nm, and the column temperature is 40 to 60 DEG C. The analysis method provided by the invention is high in specificity; the separation degree of each absorption peak is greater than or equal to 3.57; the detection method is high in repetitiveness, and the RSD is less than or equal to 1.18 percent; the sensitivity is high; the detection limit of each impurity is 0.05 ng / mL; the method is high in accuracy and durability.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring gefitinib and its related substances by high performance liquid chromatography. Background technique [0002] Gefitinib is the first small-molecule tyrosine kinase inhibitor targeting EGFR tyrosine kinase developed by AstraZeneca for the treatment of solid tumors. It was first launched in Japan in 2002 and is used to treat other chemotherapy that is ineffective or ineffective. Locally advanced or recurrent non-small cell lung cancer suitable for chemotherapy, in May 2003, it was approved in the United States and Australia as a third-line monotherapy for advanced non-small cell lung cancer. It is the first specific target for the treatment of solid tumors. Small molecule tyrosine kinase inhibitors. Launched in China in February 2005, it is suitable for the treatment of locally advanced or metastatic non-small cell lung cancer that has previously ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 杨谋伟朱素华薛峪泉张峰
Owner NANJING YOKO PHARMA
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