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Ultra-high performance liquid chromatography analysis method of clozapine related substances

An ultra-high performance liquid phase and chromatographic analysis technology, applied in the field of analysis of the purity of chemical drugs, can solve the problems of no relevant literature reports and long detection time, and achieve the effect of great positive progress and great practical application value

Active Publication Date: 2020-07-14
CHANGZHOU PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the existing pharmacopoeia documents are all common liquid phase methods, and the detection time is relatively long
[0009] Based on comprehensive impurity profile analysis, there is no relevant literature report on the analysis method of related substances in clozapine raw materials and its preparations

Method used

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  • Ultra-high performance liquid chromatography analysis method of clozapine related substances
  • Ultra-high performance liquid chromatography analysis method of clozapine related substances
  • Ultra-high performance liquid chromatography analysis method of clozapine related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: detection instrument and chromatographic conditions:

[0032] Ultra-Performance Liquid Chromatography: Waters UPLC AcQuity H-Class

[0033] Chromatographic column: Agilent Rapid Resolution HD column, specification 150×2.1mm, 1.8μm

[0034] Mobile phase A: methanol-buffer salt with a volume ratio of 25:75 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.40 with phosphoric acid);

[0035] Mobile phase B: methanol-buffer salt with a volume ratio of 90:10 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.40 with phosphoric acid);

[0036] Detection wavelength: 257nm;

[0037] Flow rate: 0.35ml / min

[0038] Column temperature: 35°C

[0039] Gradient elution program:

[0040]

[0041]

[0042] Step 1, preparation of the test solution: take clozapine 75mg in a 100ml volumetric flask, add 80ml of methanol and dilute to the mark with water, shake up as the test solution.

...

Embodiment 2

[0045] Embodiment 2: detection instrument and chromatographic conditions:

[0046] Ultra-Performance Liquid Chromatography: Waters UPLC AcQuity H-Class

[0047] Chromatographic column: Agilent Rapid Resolution HD column, specification 150×2.1mm, 1.8μm

[0048] Mobile phase A: methanol-buffer salt with a volume ratio of 25:75 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.35 with phosphoric acid);

[0049] Mobile phase B: methanol-buffer salt with a volume ratio of 90:10 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.35 with phosphoric acid);

[0050] Detection wavelength: 255nm;

[0051] Flow rate: 0.33ml / min

[0052] Column temperature: 33°C

[0053] The test results are attached image 3 .

Embodiment 3

[0054] Embodiment 3: detection instrument and chromatographic conditions:

[0055] Ultra-Performance Liquid Chromatography: Waters UPLC AcQuity H-Class

[0056] Chromatographic column: Agilent Rapid Resolution HD column, specification 150×2.1mm, 1.8μm

[0057] Mobile phase A: methanol-buffer salt with a volume ratio of 25:75 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.45 with phosphoric acid);

[0058] Mobile phase B: methanol-buffer salt with a volume ratio of 90:10 (2.0g anhydrous potassium dihydrogen phosphate, add 1000ml water to dissolve, adjust pH 2.45 with phosphoric acid);

[0059] Detection wavelength: 259nm;

[0060] Flow rate: 0.37ml / min

[0061] Column temperature: 37°C

[0062] The test results are attached Figure 4 .

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Abstract

The invention discloses an ultra-high performance liquid chromatography analysis method of clozapine. The method comprises the following steps: carrying out gradient elution by using a Waters UPLC (Ultra Performance Liquid Chromatography) AcQuity H-Class, adopting an Agilent Rapid Response HD column and taking methanol-potassium dihydrogen phosphate-water as a mobile phase. According to the method, all known impurities in the clozapine raw material and the preparation thereof can be analyzed at the same time, the content of the known impurities can be effectively controlled through a main component self-control method with correction factors, and the separation degree between a main peak and adjacent impurity peaks and the separation degree between all impurity peaks are larger than 1.5. The method is simple, short in time and accurate in impurity analysis, and a reliable analysis method is provided for clozapine.

Description

technical field [0001] The invention relates to an analysis method for the purity of chemical drugs, in particular to an ultra-high performance liquid chromatography analysis method for clozapine-related substances. Background technique [0002] Clozapine (Clozapine), the chemical name is 8-chloro-11-(4-methyl-1-piperazinyl)-5H-dibenzo[b,e][1,4]diazepine , whose structure is as follows: [0003] [0004] Clozapine is the first atypical psychiatric treatment drug. It was launched in Sweden and the United States successively in 1989 and 1990. It has small extrapyramidal adverse reactions, is effective for refractory schizophrenia and violent behavior of schizophrenia patients, and can reduce hospitalization of patients. rate and reduce treatment costs. [0005] At present, the method for synthesizing clozapine (Chinese Journal of Pharmaceutical Industry, 2013, 44 (10)) is to carry out Ullmann condensation reaction of 2,5-dichloronitrobenzene and anthranilic acid to obtai...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34
Inventor 朱怡君邱荣荣杨志明孙忠华孙光祥王兵
Owner CHANGZHOU PHARMA FACTORY
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