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Method for separating and measuring bilastine and technical impurities in preparation of bilastine

A technology of process impurities and preparations, applied in the field of analytical chemistry, can solve the problems of time-consuming, etc., and achieve the effect of quality control and shortened separation time

Active Publication Date: 2016-02-10
CHONGQING HUAPONT PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention patent with the application number 201310267146.8 discloses a method for the separation and determination of bilastine raw materials and its preparations by liquid chromatography. The related substances separated and determined mainly include four intermediates and two impurities (see the application number for the structural formula It is the background technology part of the 201310267146.8 invention patent), in which the disclosed impurity 1 has the same structure as the above-mentioned impurity F, and the rest are different; and in this patent, four intermediates and two impurities are completely separated by high performance liquid chromatography It takes 70 minutes, which is too long
At present, there is no method that can quickly and simultaneously separate the 6 impurities recorded in the above table

Method used

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  • Method for separating and measuring bilastine and technical impurities in preparation of bilastine
  • Method for separating and measuring bilastine and technical impurities in preparation of bilastine
  • Method for separating and measuring bilastine and technical impurities in preparation of bilastine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Preparation of the mixed solution: Weigh about 40mg of the test product, put it in a 25ml measuring bottle, precisely pipette 2.5ml of the impurity A-F reference substance solution, put it in the same measuring bottle as above, add diluent to dissolve and dilute to the mark, shake well, Instantly.

[0049] The diluent and the mixed solution were respectively injected according to the above-mentioned chromatographic conditions, and the chromatogram was recorded. The measurement results are shown in Table 2. see results figure 1 , figure 2 .

[0050] Table 2 test results

[0051]

[0052] Conclusion: The blank diluent does not interfere with the sample determination; the separation between the main peak and adjacent impurity peaks is greater than 1.5; the separation between the known impurity peaks is greater than 1.5; the above tests prove that the main peak and impurity peaks are well separated and specific.

[0053] comparative example

[0054] In this comparat...

Embodiment 2

[0059] Get need testing solution, sample injection by chromatographic conditions in embodiment 1, record chromatogram, and carry out blank adjuvant test in the same way, the results are shown in image 3 , Figure 4 .

[0060] Conclusion: blank excipients do not interfere with the determination of this product, indicating that the method of the present invention can be used for the quality detection of bilastine tablets.

[0061] Embodiment 3 Bilastine oxidative degradation product determination

[0062] Take 40mg of bilastine, weigh it accurately, put it in a 25ml measuring bottle, add 2.0ml of 3% hydrogen peroxide, bathe in water at 30°C for 1.5h, take it out, cool it, dissolve it with a diluent and dilute to the mark, shake it up, and measure it as a degradation product with solution.

Embodiment 3

[0063] Get the above-mentioned degradation product measurement solution, sample injection by the chromatographic conditions in Example 1, record the chromatogram, do blank test simultaneously, record the chromatogram, as Figure 5 As shown, the impurity content was calculated according to the area normalization method. The test results are shown in Table 3.

[0064] Table 3 Oxidative Degradation Test Determination Results

[0065]

[0066] Conclusion: Under the condition of oxidative degradation, impurity E was produced in 30℃ water bath for 1.5h, the level was 2.16%, and the original impurity had no change trend. The separation between the main peak and adjacent impurity peaks was greater than 1.5, and the purity factor of the main peak was 0.9999. This shows that the chromatographic conditions are good for the separation of oxidative degradation products.

[0067] Example 4 Basic research on detection limit and quantitative limit of bilastine and impurities A-F in chro...

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Abstract

The invention belongs to the field of analytical chemistry, relates to a method for separating and measuring bilastine and technical impurities in a preparation of bilastine, and specifically relates to a method for separating and measuring bilastine and six technical impurities A-F (including a degradation product) in the preparation of bilastine by adopting high performance liquid chromatography. An adopted chromatographic column takes octylsilane bonded silicone as a filler, and adopts an inorganic salt buffer system with an ion-pairing agent added and an organic solvent, wherein the inorganic salt buffer system and the organic solvent is according to a certain ratio, as a moving phase for gradient elution. According to the method, the technical impurities A-F of bilastine and the degradation product can be totally separated. The method is simple to operate and good in reproducibility. The content of a raw medicine of bilastine and relevant materials in the preparation can be effectively measured, and the method is good in specificity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a method for separating and measuring six kinds of process impurities A-F (including a degradation product) in bilastine and its preparations by using high performance liquid chromatography. Background technique [0002] Bilastine is the second generation of histamine H developed by Spanish FAES pharmaceutical company 1 Receptor antagonist, approved by the European Union in 2010 for the treatment of allergic rhinitis and chronic idiopathic urticaria. This product is safe, without the sedative effect and cardiotoxicity of commonly used antihistamines. Bilastine chemical name 2-[4-(2-(4-(1-(2-ethoxyethyl)benzimidazol-2-yl)piperidin-1-yl)ethyl)phenyl] -2-Methylpropionic acid, the molecular formula is C 28 h 37 N 3 o 3 . Bilastine structural formula is: [0003] [0004] Generally speaking, the total content of a drug impurity should be less than 0.3%, and th...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 唐舒棠沈红梅李力
Owner CHONGQING HUAPONT PHARMA
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