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Analysis and detection method for impurity in lapatinib ditosylate bulk drug

A technology of di-p-toluenesulfonic acid and lapatinib, which is applied in the direction of material separation, analytical materials, measuring devices, etc., can solve the problems that the analysis and detection methods need to be improved, and achieve good separation, good resolution, and strong specificity Effect

Inactive Publication Date: 2016-04-27
HUMANWELL HEALTHCARE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, at present, the analysis and detection method of impurities (or related substances) in lapatinib di-p-toluenesulfonate crude drug still needs to be improved

Method used

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  • Analysis and detection method for impurity in lapatinib ditosylate bulk drug
  • Analysis and detection method for impurity in lapatinib ditosylate bulk drug
  • Analysis and detection method for impurity in lapatinib ditosylate bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: the determination of detection wavelength

[0042] Get an appropriate amount of lapatinib di-p-toluenesulfonate crude drug, adopt acetonitrile-water (volume ratio 4:1) mixed solvent to dissolve and dilute to make the solution that contains about 20 μ g crude drug in every 1ml, in ultraviolet-visible spectrophotometer Full scan at 190nm~400nm, see UV scan figure 1 . Depend on figure 1 It can be seen that the maximum absorption wavelength of lapatinib di-p-toluenesulfonate is 262nm, so 262±2nm is selected as the detection wavelength.

Embodiment 2

[0044] Chromatographic conditions: 100mm×4.6mm, 3μm PhenmonexLunaC 18 Column, with 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 B, detection wavelength 262nm , the column temperature is 40 degrees Celsius, the flow rate is 10ml / min, the injection is 5μl, and the linear gradient elution gradient conditions are as follows.

[0045] time (min)

Mobile Phase A(%V / V)

Mobile Phase B(%V / V)

0

60

40

8

42

58

19

10

90

35

10

90

35.1

60

40

42

60

40

[0046] Experimental steps:

[0047] 1. Take an appropriate amount of lapatinib di-p-toluenesulfonate, dissolve it with acetonitrile-water (volume ratio 4:1) mixture and quantitatively dilute it with acetonitrile-water (volume ratio 4:1) to make 1ml containing...

Embodiment 3

[0051] In order to improve the detection limit of impurities and the resolution between impurities, the chromatographic conditions are as follows:

[0052] Using 100mm×4.6mm, 3μm PhenmonexLunaC 18 Column, with 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 B, detection wavelength 262nm , the column temperature is 40 degrees Celsius, the flow rate is 1.0ml / min, the injection volume is 15μl, and the linear gradient elution gradient conditions are shown in the table below.

[0053] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

65

35

13

65

35

[0054] 33

42

58

43

10

90

48

10

90

50

65

35

60

65

35

[0055] Experimental steps:

[0056] 1. Take an appropriate amount of...

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PUM

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Abstract

The invention provides an analysis and detection method for impurity in a lapatinib ditosylate bulk drug. The method is carried out by combining high performance liquid chromatography of an ultraviolet detector, wherein, an octadecylsilane bonded silica gel column is employed; a mobile phase is composed of a mobile phase A and a mobile phase B; a buffer salting liquid is taken as the mobile phase A, the buffer salting liquid is a phosphate solution or an acetate solution; an organic solvent is employed as the mobile phase B, the organic solvent is selected from at least one of methanol, acetonitrile and ethanol; and an elution mode is linear elution. The method can separate lapatinib ditosylate and degrade impurity introduced in a synthesis process in a good mode, and has the advantages of high sensitivity and strong specialization.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for analyzing and detecting impurities in lapatinib di-p-toluenesulfonate crude drug. Background technique [0002] Lapatinib di-toluenesulfonate is a small molecule kinase inhibitor that can simultaneously target human epidermal growth factor receptor (EGFR) and human epidermal growth factor receptor-2 (HER2), developed by GlaxoSmithKline UK Developed by the company, it was approved by the US FDA in March 2007. It is used for combination therapy: combined with capecitabine to treat advanced or metastatic breast cancer that overexpresses HER2, and combined with letrozole to treat HER2-overexpressed, hormone receptor-positive metastases breast cancer in menopausal women. [0003] However, the current analysis and detection methods for impurities (or related substances) in lapatinib di-p-toluenesulfonate bulk drug still need to be improved. Contents of the inventi...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 王学海李莉娥许勇郭涤亮夏亚子乐洋黄璐胡斌胡虹田华冯权武朱垒肖强黄松
Owner HUMANWELL HEALTHCARE GRP
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