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A method for separating and measuring process impurities in bilastine and its preparations

A technology for process impurities and preparations, applied in the field of analytical chemistry, can solve problems such as time-consuming and achieve the effect of controllable quality and shortening of separation time

Active Publication Date: 2019-04-16
CHONGQING HUAPONT PHARMA
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  • Summary
  • 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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  • A method for separating and measuring process impurities in bilastine and its preparations
  • A method for separating and measuring process impurities in bilastine and its preparations
  • A method for separating and measuring process impurities in bilastine and its preparations

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The chromatogram of embodiment 1 bilastine and 6 kinds of process impurities

[0047] Preparation of impurity A-F reference substance solution: Take about 40 mg of impurity A-F reference substance respectively, put them in a 25ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well to obtain impurity A-F stock solution. Precisely pipette 0.5ml of each of the above solutions, put them in a 50ml measuring bottle, add diluent to dilute to the mark, and shake well to obtain a reference substance mixture with a concentration of impurities A-F of 20 μg / ml.

[0048] Preparation of the mixed solution: Weigh about 40mg of the test product, put it in a 25ml measuring bottle, precisely pipette 2.5ml each 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 ...

Embodiment 2

[0057] Example 2 The impact of bilastine tablet preparation excipients on the determination of bilastine

[0058] Take an appropriate amount of bilastine tablets (including 40mg bilastine), put it in a 25ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, filter, and take the filtrate as the test solution.

[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.

Embodiment 3

[0061] Example 3 Determination of Bilastine Oxidative Degradation Products

[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.

[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 Determination results of oxidative degradation test

[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...

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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 t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 唐舒棠沈红梅李力
Owner CHONGQING HUAPONT PHARMA
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