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Method for detecting sorafenib-tosylate-related substances

A technology related to substances and detection methods, applied in the field of analytical chemistry, can solve problems such as poor resolution, impurity inspection, system applicability, repeatability, linear range, quantitative limit and detection limit difference, etc., to achieve high system adaptability, The effect of high precision and high peak symmetry

Inactive Publication Date: 2016-12-14
HEFEI HUAFANG PHARMA SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Also refer to relevant literature, using pH 2.4 phosphate buffer salt-acetonitrile-ethanol gradient elution, but the separation between the p-toluenesulfonic acid peak and the impurity A peak, between the main peak and its adjacent impurity F peak before the peak is poor, affecting the impurity check
The existing detection methods are poor in system applicability, repeatability, linear range, limit of quantification, limit of detection, etc. due to poor chromatographic conditions and methods

Method used

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  • Method for detecting sorafenib-tosylate-related substances
  • Method for detecting sorafenib-tosylate-related substances
  • Method for detecting sorafenib-tosylate-related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: chromatographic conditions and chromatographic system of detection method of the present invention

[0041] Instrument: Shimadzu high performance liquid chromatography

[0042] Chromatographic column: Waters Symmetry C18 (4.6×100mm, 3.5μm)

[0043] Mobile phase A: pH3.0 phosphate buffer (take 2.72g potassium dihydrogen phosphate, add water to dissolve and dilute to 1000ml, adjust the pH value to 3.0 with phosphoric acid); mobile phase B: acetonitrile:ethanol=60:40; detection wavelength : 250nm; Flow rate: 1.0ml / min; Injection volume: 20μl; Column temperature: 35℃

[0044] Table 1: Elution Program

[0045] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

65

35

10

50

50

26

50

50

27

65

35

45

65

35

[0046] Preparation of the test solution: Get about 27.4 mg of Sorafenib tosylate, put it in a 100ml measuring bottle, add an appropriate amount of mixed solution, ultrasonical...

Embodiment 2

[0049] Embodiment 2: detection method system applicability detection of the present invention

[0050] Diluent: mobile phase A-mobile phase B (1:3) (V / V); blank solution: diluent

[0051] Impurity stock solution: Take about 20 mg each of impurity A, impurity B, impurity C, impurity D, impurity E and impurity F, weigh them accurately, put them in a 100ml measuring bottle, add an appropriate amount of diluent, dissolve them by ultrasonic, let cool, and dilute with Dilute to the mark with diluent, shake well, accurately measure 5ml, put it in a 50ml measuring bottle, dilute to the mark with diluent, shake well, and use it as the reference substance stock solution;

[0052] System suitability test solution: take another about 27.5 mg of sorafenib tosylate reference substance, accurately weigh it, put it in a 100ml measuring bottle, add an appropriate amount of diluent, dissolve it by ultrasonication, then precisely add 1ml of the above stock solution, and dilute it with Dilute th...

Embodiment 3

[0057] Embodiment 3: Specific detection of the detection method of the present invention

[0058] The strong degradation test is to simulate the strong degradation conditions of strong acid, strong alkali, oxidation, high temperature and light to destroy sorafenib tosylate. The effectiveness and applicability of the analytical method can be evaluated by comparing the amount of impurity generated with the reduction of the main component. At the same time, the DAD detector is used to check the peak purity: in the spectrum obtained from the degradation test, when the purity factor of the main component is greater than the threshold, it can be judged that the chromatographic peak does not contain other impurity peaks, and the chromatographic peak purity meets the requirements. The specific test results are shown in the table 4. The corresponding chromatogram instructions are attached Figure 3-8 .

[0059] Table 4: Specificity test results

[0060]

[0061] According to the ...

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Abstract

The invention relates to the field of analytical chemistry, and particularly discloses a method for detecting sorafenib-tosylate-related substances. The detecting method includes the steps that a to-be-tested sorafenib-tosylate product is taken to prepare a test solution, and the test solution is diluted by one hundred times to serve as a contrast solution; then a pH3.0 phosphate buffer solution (1.36 g of monopotassium phosphate is taken, dissolved with water and diluted to 1000 ml, and the pH value is adjusted to be 3.0 with phosphoric acid) serves as a mobile phase A, acetonitrile-ethanol (60:40) serves as a mobile phase B, and gradient eluting is carried out according to the following table, wherein the detection wavelength is 250 nm, and the column temperature is 35 DEG C; HPLC detection is carried out, and the content of the related substances is measured according to the correction-factor-added main-constituent self-contrast method. According to the method, the acetonitrile-ethanol phosphate-buffer-solution gradient elution system is adopted, the chromatographic peak of sorafenib tosylate can have the higher separation degree than that of other related substances and high peak-pattern symmetry, the related substances can be detected, and high system suitability is achieved; meanwhile, incomparable advantages are shown in the specificity, the quantitation limit, the detection limit, the linear range and the repeatability, and high precise is achieved.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting related substances of Sola toluenesulfonate. Background technique [0002] Sorafenib tosylate, English name Sorafenib Tosylate, is indicated for the treatment of inoperable advanced renal cell carcinoma; the treatment of inoperable or distantly metastatic primary hepatocellular carcinoma. According to our previous research and development experience, the main known related substances of sorafenib tosylate are impurity A, impurity B, impurity C, impurity D, impurity E, impurity F, impurity G and impurity H, which come from synthetic raw materials, Intermediates and degradation products, the structural formula is as follows: [0003] [0004] [0005] In view of the current strict requirements for sorafenib tosylate products, after the synthesis of sorafenib tosylate, the content of related substances needs to be tested in order to meet the standard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 陈丽何勇高永好吴宗好彭扶云
Owner HEFEI HUAFANG PHARMA SCI & TECH
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