An analytical method for detecting related substances of gefitinib

An analytical method and a chromatographic technique, which are applied in the field of analysis of the detection of gefitinib-related substances, can solve the problems of complex preparation process, inability to separate, and difficult separation of gefitinib, and achieve good separation and low detection limit , good separation effect

Active Publication Date: 2022-05-24
NANJING SHUNXIN PHARM CO LTD OF CHIATAI TIANQING PHARM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The preparation process of gefitinib is complicated, the impurities are various, and the separation is difficult. The current impurity analysis methods have different problems in terms of system applicability, ease of use, economy, and separation effects. For example, the common high-efficiency liquid Phase chromatography cannot separate related substance formula 7 compound and gefitinib

Method used

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  • An analytical method for detecting related substances of gefitinib
  • An analytical method for detecting related substances of gefitinib
  • An analytical method for detecting related substances of gefitinib

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Example 1 Exclusive detection method for compound of formula 7 in gefitinib.

[0072] Solvent: Methanol.

[0073] Mobile phase B: Weigh 1.54 g of ammonium acetate, add 1 L of methanol, and ultrasonically mix to obtain a 20 mmol / L ammonium acetate methanol solution as mobile phase B.

[0074] Gefitinib crude product test solution: Weigh 10 mg of gefitinib crude product, put it in a 10 mL measuring bottle, add methanol to dissolve and dilute to the scale, mix well, and obtain.

[0075] Gefitinib test solution: Weigh 10mg of Gefitinib, put it in a 10mL measuring bottle, add methanol to dissolve and dilute to the mark, mix well, and obtain.

[0076] Impurity stock solution: Weigh 25mg of the compound of formula 7, put it in a 25mL measuring bottle, add methanol to dissolve and dilute to the mark, accurately measure 1mL, put it in a 100mL measuring bottle, dilute to the mark with methanol, and mix well to get ready.

[0077] Impurity reference substance solution: Accuratel...

Embodiment 2

[0086] Example 2 Quantitation limit and detection limit test of the compound of formula 7.

[0087] Solvent: Methanol.

[0088] Mobile phase B: Weigh 1.54 g of ammonium acetate, add 1 L of methanol, and ultrasonically mix to obtain a 20 mmol / L ammonium acetate methanol solution as mobile phase B.

[0089] Detection limit detection solution: Take 1mL of the impurity stock solution in the specificity test, put it in a 20mL measuring bottle, dilute to the mark with methanol, mix well, and get ready.

[0090] Quantitation limit detection solution: Take 2mL of the impurity stock solution in the specificity test, put it in a 10mL measuring bottle, dilute with methanol to the mark, mix well, and get ready.

[0091] According to the test of supercritical fluid chromatography (Chinese Pharmacopoeia 2015 Edition Sibu General Rules 0531), use ethylene bridge hybrid particles as filler (recommended use: Waters Torus 2-PIC (3.0×100mm, 1.7μm)); 2 It is the mobile phase A, 20mmol / L ammoniu...

Embodiment 3

[0098] Example 3 The compound of formula 7 in gefitinib was separated and detected by HPLC.

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Abstract

The invention relates to an analytical method for detecting gefitinib related substances, and belongs to the field of pharmaceutical analytical chemistry. Specifically relate to a kind of detection gefitinib crude product and related substance in finished product is N-(3-chloro-4-fluorophenyl)-7-(3-morpholine-4-propoxy) quinazoline- Analytical Methods for 6-Methoxy-4-Amine. Common high performance liquid chromatography cannot separate the related substance and gefitinib. The application provides a method for detecting the related substance in gefitinib by supercritical fluid chromatography. The separation effect between the impurity peak and the gefitinib peak is good, the sensitivity and accuracy are high, the acquisition time is short, and the specificity is high, which can better control the product quality of gefitinib.

Description

technical field [0001] The invention belongs to the field of pharmaceutical analytical chemistry, and relates to an analytical method for detecting related substances of gefitinib, in particular to a method for detecting that the related substances in crude and finished products of gefitinib are N-(3-chloro-4-fluorophenyl )-7-(3-morpholine-4-propoxy)quinazolin-6-methoxy-4-amine analysis method. Background technique [0002] Gefitinib (Gefitinib) is a selective epidermal growth factor receptor (EGFR) tyrosine kinase inhibitor developed by AstraZeneca Pharmaceuticals Co., Ltd., suitable for epidermal growth factor receptor (EGFR) gene with sensitivity First-line treatment of patients with locally advanced or metastatic non-small cell lung cancer (NSCLC) with mutations and for the treatment of locally advanced or metastatic non-small cell lung cancer (NSCLC) who have previously received chemotherapy. The chemical name of gefitinib is N-(3-chloro-4-fluorophenyl)-7-methoxy-6-(3-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/8675Y02P20/55Y02P20/54
Inventor 周玉洁江金凤陈智林郝锐张喜全顾红梅史晋辉郭猛王勇刘金虎
Owner NANJING SHUNXIN PHARM CO LTD OF CHIATAI TIANQING PHARM GRP
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