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A kind of ultra-high performance liquid chromatography analysis method of clozapine related substances

An ultra-high performance liquid chromatography 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, long detection time, etc.

Active Publication Date: 2022-07-12
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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  • A kind of ultra-high performance liquid chromatography analysis method of clozapine related substances
  • A kind of ultra-high performance liquid chromatography analysis method of clozapine related substances
  • A kind of ultra-high performance liquid chromatography analysis method of clozapine related substances

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Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0032] UPLC: Waters UPLC AcQuity H-Class

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

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

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

[0036] Detection wavelength: 257nm;

[0037] Flow rate: 0.35ml / min

[0038] Column temperature: 35℃

[0039] Gradient elution procedure:

[0040]

[0041]

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

[0043...

Embodiment 2

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

[0046] UPLC: Waters UPLC AcQuity H-Class

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

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

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

[0050] Detection wavelength: 255nm;

[0051] Flow rate: 0.33ml / min

[0052] Column temperature: 33℃

[0053] The test results are attached image 3 .

Embodiment 3

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

[0055] UPLC: Waters UPLC AcQuity H-Class

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

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

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

[0059] Detection wavelength: 259nm;

[0060] Flow rate: 0.37ml / min

[0061] Column temperature: 37℃

[0062] The test results are attached Figure 4 .

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Abstract

The invention discloses an ultra-high performance liquid chromatography analysis method for clozapine, which uses Waters UPLC AcQuity H-Class, adopts Agilent Rapid Resolution HD column, and uses methanol-potassium dihydrogen phosphate-water as mobile phase to carry out gradient elution. This method can simultaneously analyze all known impurities in clozapine raw materials and their preparations, and can effectively control the content of known impurities through the main component self-contrast method with correction factor, the main peak and adjacent impurity peaks and the difference between each impurity peak. The degree of separation was greater than 1.5. The method is simple, time-consuming and accurate in impurity analysis, providing a reliable analytical method for clozapine.

Description

technical field [0001] The invention relates to a method for analyzing the purity of chemical drugs, in particular to an ultra-high performance liquid chromatography method for analyzing clozapine related substances. Background technique [0002] Clozapine (Clozapine), chemical name is 8-chloro-11-(4-methyl-1-piperazinyl)-5H-dibenzo[b,e][1,4]diazepine , and its structural formula is as follows: [0003] [0004] Clozapine is the first atypical psychiatric drug. It was launched in Sweden and the United States in 1989 and 1990. It has few extrapyramidal adverse reactions, is effective in treating refractory schizophrenia and violent behavior in patients with schizophrenia, and can reduce hospitalization. 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 with 2,5-dichloronitrobenzene and anthranilic acid to obtain 2-(4-chloro- ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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