Method for Determination of Related Substances of Ebastine by High Performance Liquid Chromatography

A high-performance liquid chromatography and ebastine technology, which is applied in the field of high-performance liquid chromatography for the determination of ebastine related substances, can solve the problems of tailing, unfavorable popularization and application, inconvenient measurement, and saves detection time. , The effect of high detection accuracy and shortened cycle time

Active Publication Date: 2015-10-14
JIANGSU LIANHUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] European Pharmacopoeia (EP8.0), using acetonitrile-phosphoric acid-sodium hydroxide solution (pH5.0) for isocratic elution, the analysis time period is as long as 3 hours, the main peak emerges in about 110 minutes, and the tailing is serious, the determination is very difficult Inconvenient, not conducive to the actual promotion and application;
[0006] The national drug standard method uses methanol-ammonium acetate buffer (pH3.9) as the mobile phase, and the detection wavelength is 254nm, but some impurities have no absorption at this wavelength, and the impurities cannot be effectively separated, and the impurities cannot be accurately detected;
[0007] The method described in Chinese patent CN102095808 uses a phosphate buffer solution of triethylamine (pH6.5-10.8) as the mobile phase, and there are blunt peaks and tails, impurities that cannot be effectively separated, and impurities that cannot be completely detected at the preferred wavelength of 250nm

Method used

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  • Method for Determination of Related Substances of Ebastine by High Performance Liquid Chromatography
  • Method for Determination of Related Substances of Ebastine by High Performance Liquid Chromatography
  • Method for Determination of Related Substances of Ebastine by High Performance Liquid Chromatography

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Experimental program
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Effect test

Embodiment 1

[0076] Chromatographic conditions: mobile phase A is phosphate buffer (take 3.58g of disodium hydrogen phosphate dodecahydrate, add water to dissolve and dilute to 1000ml, adjust the pH value to 6.3 with phosphoric acid, add 1.92g of sodium lauryl sulfate, mix well )-acetonitrile=80:20, mobile phase B is acetonitrile; flow rate: 1.0ml / min; perform linear gradient elution according to Table 1.

[0077] Preparation of the test sample solution: take an appropriate amount of this product, add a solvent to dissolve and dilute to make a solution containing 2.0 mg of ebastine per 1 ml, as the test sample solution; accurately measure the test sample solution in an appropriate amount, dilute with a solvent to prepare A solution containing 2 μg of ebastine per 1 ml was used as a control solution. Inject the sample and record the chromatogram.

[0078] Test results such as figure 1 shown. figure 1 Among them, the 8 kinds of impurities in the ebastine raw material drug were completely ...

Embodiment 2-3

[0080] Chromatographic conditions: mobile phase A is phosphate buffer [take (Example 2-dipotassium hydrogen phosphate 2.28g), (Example 3-diammonium hydrogen phosphate 1.32g), add water to dissolve and dilute to 1000ml, adjust pH with phosphoric acid value to 6.3, add 1.92g of sodium lauryl sulfate, mix]-acetonitrile (80:20), mobile phase B is acetonitrile; flow rate: 1.0ml / min; linear gradient elution as listed in Table 1.

[0081] Preparation of the test solution: take an appropriate amount of this product, add solvent to dissolve and dilute to make a solution containing about 2.0 mg of ebastine per 1 ml, as the test solution; accurately measure the appropriate amount of the test solution, and dilute it with a solvent Prepare a solution containing about 2 μg of ebastine per 1 ml as a control solution. Inject the sample and record the chromatogram.

[0082] Embodiment 2 result sees attached figure 2 ; Embodiment 3 results are attached image 3 . pass figure 2 , image ...

Embodiment 4-5

[0084] Chromatographic conditions: mobile phase A is phosphate buffer (1.79g of disodium hydrogen phosphate dodecahydrate is taken in embodiment 4, 17.9g of disodium hydrogen phosphate dodecahydrate is taken in embodiment 5, dissolved in water and diluted to 1000ml, adjusted with phosphoric acid When the pH value reaches 6.3, add 1.92 g of sodium lauryl sulfate, mix well)-acetonitrile (80:20), mobile phase B is acetonitrile; flow rate: 1.0ml / min; perform linear gradient elution as listed in Table 1.

[0085] Preparation of the test solution: take an appropriate amount of this product, add solvent to dissolve and dilute to make a solution containing about 2.0 mg of ebastine per 1 ml, as the test solution; accurately measure the appropriate amount of the test solution, and dilute it with a solvent Prepare a solution containing about 2 μg of ebastine per 1 ml as a control solution. Inject the sample and record the chromatogram.

[0086] Embodiment 4 result sees attached Figure...

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Abstract

The invention provides a method for testing ebastine-related substances by high performance liquid chromatography. The method includes: a, preparing a sample solution for test: preparing the sample solution for test by mixing a to-be-tested sample with a solvent; b, testing: testing the sample solution at the test wavelength of 200-220 nanometers by a gradient elute method by means of utilizing octadecylsilane chemically bonded silica as a chromatographic column filler, utilizing mixed liquid of a phosphate buffered solution and an organic solvent as a moving phase A and utilizing the organic solvent as a moving phase B. The method for testing the ebastine-related substances by the high performance liquid chromatography has the advantage that related substances in ebastine active ingredients can be separated and tested quickly, effectively, accurately and reliably.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for determining related substances of ebastine by high performance liquid chromatography. Background technique [0002] Ebastine, chemical name: 1-[4-(1,1-dimethylethyl)phenyl]-4-[4-(diphenylmethoxy)-1-piperidine Base]-1-butanone is a group of amine H1 receptor blockers, which are widely used in the treatment of urticaria, allergic rhinitis, eczema and other treatments. [0003] The composition of ebastine API is clear, mainly including ebastine and 8 kinds of related impurities. It is very important to separate these 9 kinds of substances thoroughly and quickly. [0004] Existing high performance liquid phase analysis methods for related substances of ebastine include: [0005] European Pharmacopoeia (EP8.0), using acetonitrile-phosphoric acid-sodium hydroxide solution (pH5.0) for isocratic elution, the analysis time period is as long as 3 hours, the main peak emerges in abou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 扈田进张德伟褚青松郭蕾贾志祥秦雄剑
Owner JIANGSU LIANHUAN PHARMA
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