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Detection method of olopatadine hydrochloride and related substance thereof

A technology of olopatadine hydrochloride and a detection method, applied in the field of analysis and detection, can solve the problems of not fully reflecting the product quality, the safety risk of clinical drug use, the small amount of impurities, etc., so as to reduce the risk of clinical drug use, have high sensitivity, and improve accuracy sexual effect

Active Publication Date: 2020-03-06
北京海晶生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The detection method of related substances of olopatadine hydrochloride is recorded in United States Pharmacopoeia USP41 and Japanese Pharmacopoeia JP17, and the applicant finds through tests that the detection method of related substances of olopatadine hydrochloride recorded in USP41 and JP17, due to wavelength, For reasons such as gradient and flow, the number of impurities that can be detected is small, which cannot fully reflect the quality of the product, and brings potential safety risks to clinical medication.

Method used

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  • Detection method of olopatadine hydrochloride and related substance thereof
  • Detection method of olopatadine hydrochloride and related substance thereof
  • Detection method of olopatadine hydrochloride and related substance thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Test sample solution: Weigh 50mg of olopatadine hydrochloride sample to be tested, put it in a 100ml measuring bottle, add a diluent, dissolve it ultrasonically, then set the volume to the mark, shake well and filter to get it; the diluent is: volume ratio It is a 3:2 mixed solution of 0.05mol / L phosphate buffer solution (pH3.5) and acetonitrile.

[0040] Get the test sample solution, inject it into the liquid chromatograph, record the chromatogram, and complete the determination. The resulting chromatogram is as follows: figure 1 Shown, impurity result analysis is shown in Table 2.

[0041] The detection method is: the detection method of olopatadine hydrochloride and related substances specified in JP17, and the specific detection conditions are as follows:

[0042] Testing instrument: Shimadzu LC-20AT high performance liquid chromatography;

[0043] Wavelength: 299nm;

[0044] Chromatographic column: C8, 250×4.6mm, 5μm;

[0045] Injection volume: 30μl;

[0046] ...

Embodiment 2

[0053] Test sample solution: Weigh 20 mg of the same batch of olopatadine hydrochloride to be tested in Example 1, put it in a 100ml measuring bottle, add a diluent, dissolve it ultrasonically, then set the volume to the mark, shake well and filter to obtain the solution. Wherein the diluent is the mobile phase.

[0054] Get the test sample solution, inject it into the liquid chromatograph, record the chromatogram, and complete the determination. The resulting chromatogram is as follows: figure 2 Shown, impurity result analysis is as shown in table 3.

[0055] The detection method is: the detection method of olopatadine hydrochloride and related substances specified in USP41, and the specific detection conditions are as follows:

[0056] Detection instrument: Agilent 1260 high performance liquid chromatography;

[0057] Wavelength: 299nm;

[0058] Chromatographic column: C8, 150×4.6mm, 5μm;

[0059] Flow rate: 1.0ml / min;

[0060] Injection volume: 30μl;

[0061] Column ...

Embodiment 3

[0068] Test sample solution: Weigh 20 mg of the same batch of olopatadine hydrochloride sample to be tested as in Example 1, put it in a 100ml measuring bottle, add a diluent, dissolve it ultrasonically, then set the volume to the mark, shake well and filter to obtain. Wherein the diluent is a mixed solution of mobile phase A and mobile phase B with a volume ratio of 75:25.

[0069] Get the test sample solution, inject it into the liquid chromatograph, record the chromatogram, and complete the determination. The resulting chromatogram is as follows: image 3 Shown, impurity result analysis is shown in table 4.

[0070] The specific detection conditions are as follows:

[0071] Detection instrument: Agilent 1260 high performance liquid chromatography;

[0072] Wavelength: 240nm;

[0073] Chromatographic column: C8, 150×4.6mm, 5μm;

[0074] Flow rate: 1.0ml / min;

[0075] Injection volume: 30μl;

[0076] Column temperature: 40°C;

[0077] Mobile phase A: an aqueous solutio...

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Abstract

The invention relates to a detection method of olopatadine hydrochloride and related substance thereof. The method comprises a step of using high performance liquid chromatography for detection, wherein liquid chromatographic conditions are as follows: an octyl silane bonded silica gel chromatographic column is used; a mobile phase A is aqueous solution containing 0.01%-1% ion pair reagent, 0.3%-1% monoamine and 0.001-0.1mol / L buffer salt, a mobile phase B is acetonitrile and / or methyl alcohol, and gradient eluting is executed; and a pH value of buffer solution is 2.5-3.5, and detection wavelength is 220nm-280nm. The detection method of the olopatadine hydrochloride and the related substance thereof provided by the invention can effectively separate the olopatadine hydrochloride and impurities thereof, improve accuracy of a detection result and reduce clinical medication risks.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, in particular to a detection method of olopatadine hydrochloride and related substances. Background technique [0002] The molecular formula of "olopatadine hydrochloride" is C 21 h 24 ClNO 3 , named (Z)-11-[3-(dimethylamino)propylene]-6,11-dihydrodibenzo[b,e]oxazepine-2-acetic acid hydrochloride, English The name is Olopatadine Hydrochloride, the CAS number is 140462-76-6, and the structural formula is shown in Formula 1. It is an anti-allergic drug developed and marketed by Japan Kyowa Hakka Co., Ltd. It can be used to treat allergic rhinitis and urticaria, and can improve skin diseases with itching symptoms. [0003] [0004] The detection method of related substances of olopatadine hydrochloride is recorded in United States Pharmacopoeia USP41 and Japanese Pharmacopoeia JP17, and the applicant finds through tests that the detection method of related substances of olopatad...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 曹相林李萍张鑫楠商丹丹吴绪丽
Owner 北京海晶生物医药科技有限公司
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