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Method for analyzing lapatinib ditosylate isomer impurities

A technology of di-p-toluenesulfonic acid and isomers, which is applied in the field of pharmaceutical analysis, can solve the problems that the analysis and detection methods need to be improved, and achieve the effects of short time, high separation efficiency and strong specificity

Active Publication Date: 2016-07-06
HUBEI BIO PHARMA IND TECHCAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the current analysis and detection methods for the isomer impurities of lapatinib di-p-toluenesulfonate still need to be improved

Method used

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  • Method for analyzing lapatinib ditosylate isomer impurities
  • Method for analyzing lapatinib ditosylate isomer impurities
  • Method for analyzing lapatinib ditosylate isomer impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Embodiment 1: Determination of detection wavelength

[0063] Take and add acetonitrile-water (volume ratio 4:1) mixed solvent to dissolve and dilute to make a solution containing about 20 μg of raw material per 1 ml, and perform a full scan at 190nm to 400nm on a UV-visible spectrophotometer, di-p-toluenesulfonate The UV scanning results of lapatinib acid are shown in figure 1 . Depend on figure 1 It can be seen that the maximum absorption wavelength of lapatinib di-p-toluenesulfonate is 261nm, so 261±2nm is selected as the detection wavelength.

Embodiment 2

[0065] Using PhenmonexlunaC 18 3μm, 100×4.6mm chromatographic column, use 50mmol / L ammonium acetate buffer solution (take 3.85g ammonium acetate, dissolve in 990ml water, adjust pH to 4.5 with glacial acetic acid, dilute to 1000ml with water) as mobile phase A, use acetonitrile as mobile phase Mobile phase B, the detection wavelength is 261nm, the column temperature is 40°C, and 5 μl of sample is injected, and the linear gradient elution gradient is performed according to the following table:

[0066] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

65

35

13

65

35

33

42

58

43

10

90

48

10

90

50

65

35

60

65

35

[0067] Experimental steps:

[0068] 1. Take an appropriate amount of lapatinib di-p-toluenesulfonate, dissolve it with acetonitrile-water (volume ratio 4:1) and quantitatively dilute it with acetonitrile-water (volume ratio 4:1) to make 1m...

Embodiment 3

[0072] (1) Take lapatinib di-p-toluenesulfonate bulk drug, dissolve it ultrasonically in an acetonitrile-water mixed solvent with a volume ratio of 4:1, and prepare lapatinib di-p-toluenesulfonate with a concentration of 0.1mg / ml The test solution;

[0073] Chromatographic conditions:

[0074] The instrument adopts a high-performance liquid chromatograph equipped with an ultraviolet detector; a pentafluorophenyl column PhenmonexKinetex2.6μmPFP100×4.6mm chromatographic column is used, and the ammonium acetate buffer solution with a concentration of 50mmol / L adjusted to pH 4.5 with glacial acetic acid is used as the flow Phase A, using methanol as the mobile phase B, the volume ratio of the ammonium acetate buffer and methanol is 30:70, the elution method is isocratic elution, the detection wavelength is 261nm, the flow rate is 1.0ml / min, the column The temperature is 40 degrees centigrade, and isocratic elution is carried out according to the conditions shown above;

[0075] ...

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Abstract

The invention provides a method for analyzing lapatinib isomer impurities. The method is carried out by adoption of high performance liquid chromatography combined with an ultraviolet detector. In high performance liquid chromatography, a pentafluorophenyl column is adopted; a mobile phase comprises a mobile phase A and a mobile phase B, wherein an ammonium acetate buffer solution is taken as the mobile phase A, and methanol is taken as the mobile phase B; and an isocratic elution mode is adopted. According to the method, lapatinib ditosylate isomer impurities can be well separated. The method is high in sensitivity and good in specialization, and the separation degree can reach requirements.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for analyzing the isomer impurities of lapatinib di-p-toluenesulfonate. Background technique [0002] Lapatinib di-toluenesulfonate has a structure shown in Formula 1: [0003] [0004] Lapatinib is a small molecule kinase inhibitor that can simultaneously target human epidermal growth factor receptor (EGFR) and human epidermal growth factor receptor-2 (HER2). Ni, developed by GlaxoSmithKline in the United Kingdom, was approved by the US FDA in March 2007 for combination therapy: combined use of capecitabine for the treatment of advanced or metastatic breast cancer that overexpresses HER2, and combination of letrozole for the treatment of overexpressed HER2 HER2, hormone receptor positive metastatic breast cancer in postmenopausal women. [0005] However, the current analysis and detection methods for the isomer impurities of lapatinib di-p-toluenesulfonate st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N21/33
Inventor 王学海许勇李莉娥夏亚子郭涤亮乐洋黄璐杨仲文余艳平胡斌胡虹田华冯权武朱垒肖强黄松于静
Owner HUBEI BIO PHARMA IND TECHCAL INST
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