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Method for detecting genotoxic impurity in pentoxifylline

A technology of pentoxifylline and genotoxicity, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem that the sensitivity cannot meet the detection requirements, and achieve the effect of improving sample analysis efficiency, strong specificity, and high repeatability

Active Publication Date: 2021-11-23
SHIJIAZHUANG NO 4 PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The sensitivity of conventional gas chromatography or liquid chromatography detection methods cannot meet the detection requirements of impurity D in pentoxifylline raw materials, and there are still relevant literature reports on detection methods that can meet this requirement

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  • Method for detecting genotoxic impurity in pentoxifylline
  • Method for detecting genotoxic impurity in pentoxifylline
  • Method for detecting genotoxic impurity in pentoxifylline

Examples

Experimental program
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Effect test

Embodiment 1

[0054] This embodiment provides a detection method for genotoxic impurities in pentoxifylline, the detection method comprising the following steps:

[0055] Step 1, preparing the test solution, reference solution, blank solution and mixed solution;

[0056] The preparation of above-mentioned reference substance solution: get 3-(3-chloropropoxyl)-2-enoic acid ethyl ester reference substance, be mixed with methanol the reference substance stock solution that concentration is 499.37ng / mL, then to above-mentioned reference substance storage solution was diluted to obtain a concentration of 12.5ng / mL reference substance solution;

[0057] The preparation of above-mentioned need testing solution: take need testing 100mg, accurately weigh, place 10mL volumetric flask, add methanol to dissolve and dilute to scale, as need testing solution;

[0058] Above-mentioned blank solution is methanol solvent;

[0059] Preparation of the above mixed solution: Take 100 mg of the test product and ...

Embodiment 2

[0072] Embodiment 2 detection limit and quantitative limit

[0073] Limit of detection: the reference substance solution with a concentration of 12.5 ng / mL prepared in Example 1 was quantitatively diluted step by step with methanol, and then detected by liquid chromatography-mass spectrometry. The specific conditions of liquid chromatography and mass spectrometry are as in Example 1 As mentioned above, record the spectrogram, and obtain the detection limit according to the signal-to-noise ratio not lower than 3:1, and the results are shown in Table 1.

[0074] Quantitation limit: the concentration prepared in Example 1 is that the 12.5ng / mL reference substance solution is quantitatively diluted step by step with methanol, and then the liquid chromatography-mass spectrometry method is used to detect the quantitative limit solution. The specific conditions of liquid chromatography and mass spectrometry are as follows: As described in Example 1, the spectrogram was recorded, and ...

Embodiment 3

[0080] Embodiment 3 linear relationship

[0081] The reference substance stock solution with a concentration of 499.37ng / mL prepared in Example 1 was diluted with methanol to obtain concentrations of 2.50ng / mL, 4.99ng / mL, 9.99ng / mL, 12.48ng / mL, and 19.97ng / mL respectively. , 24.97ng / mL linear solution.

[0082] The linear solution prepared above was detected by liquid chromatography-mass spectrometry. The specific conditions of liquid chromatography and mass spectrometry were as described in Example 1, and the spectra were recorded. Taking the concentration (ng / mL) of 3-(3-chloropropoxy)-2-enoic acid ethyl ester (impurity D) as the abscissa, taking the peak area as the ordinate, draw a standard curve, and calculate the regression equation, the result See Table 3, see the linear graph Figure 5 . It can be seen from the results that the impurity D has a good linear relationship within the concentration range of 2.50ng / mL-24.97ng / mL.

[0083] Table 3 impurity D linear relati...

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Abstract

The invention relates to the technical field of pharmaceutical analysis, and particularly discloses a method for detecting a genotoxic impurity in pentoxifylline. The detection method comprises the following steps that: a test solution and a reference solution are prepared; and the test solution and the reference solution are detected by adopting a liquid chromatography-mass spectrometry method. The chromatographic conditions of liquid chromatography are as follows: gradient elution is performed by adopting a C18 chromatographic column and taking a formic acid aqueous solution with the volume concentration of 0.1% as a mobile phase A and methanol as a mobile phase B; and the mass spectrometry adopts an ESI ion source and a positive ion detection mode. The detection method provided by the invention has the advantages of simplicity, stability, high precision, good reproducibility and the like, can quickly and accurately detect a genotoxic impurity D in a pentoxifylline bulk drug, and accords with the guiding principle of ICH M7.

Description

technical field [0001] The invention relates to the technical field of drug analysis, in particular to a method for detecting genotoxic impurities in pentoxifylline. Background technique [0002] Pentoxifylline is a dimethylxanthine derivative that can reduce blood viscosity, thereby improving blood fluidity, promoting microcirculation in ischemic tissues, and increasing oxygen supply to special organs. Its mechanism of action is: by inhibiting phosphodiesterase, increasing the content of intracellular adenosine triphosphate, thereby improving the deformability of red blood cells, and at the same time reducing fibrinogen, inhibiting the aggregation of red blood cells and platelets. It is mainly suitable for cerebral blood circulation disorders such as transient cerebral ischemic attack, sequelae of stroke, brain dysfunction caused by cerebral ischemia; peripheral blood circulation disorders such as thromboangiitis obliterans, etc., can protect cardiovascular and cerebrovascu...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/86
CPCG01N30/02G01N30/72G01N30/8679
Inventor 董海峰王亚静范燕龙马明卓骆会茹王肖胡硕宗莹莹韩倩茹
Owner SHIJIAZHUANG NO 4 PHARMA
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