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Liquid phase analysis method of maleic acid asenapine and impurities thereof

A technology for asenapine maleate and impurities, which is applied in the field of analytical chemistry, can solve problems such as incomplete removal of intermediates, affecting the purity and quality of drugs, and achieve the effect of ensuring quality control

Inactive Publication Date: 2015-01-21
AVENTIS PHARMA HAINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of synthesizing the compound, some important intermediates may be incompletely removed, and degradation impurities may also be produced during the transportation and storage of the compound, and these incompletely removed intermediates and degradation impurities will affect the purity and quality

Method used

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  • Liquid phase analysis method of maleic acid asenapine and impurities thereof
  • Liquid phase analysis method of maleic acid asenapine and impurities thereof
  • Liquid phase analysis method of maleic acid asenapine and impurities thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instruments and Conditions:

[0037] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0038] Column: C 8 (Apollo, 250×4.6mm, 5μm)

[0039] Mobile phase: Phase A: 0.02mol / L potassium dihydrogen phosphate buffer solution (weigh 2.72g of potassium dihydrogen phosphate, add water to dissolve and set the volume to 1000mL, adjust the pH value to 3.5 with dilute phosphoric acid), phase B: acetonitrile, using a gradient Elution;

[0040] T(min) 0 35 65 75 80 90 B% 23 30 60 60 23 23

[0041] Flow rate: 1.0mL / min

[0042] Detection wavelength: 220nm

[0043] Column temperature: 25°C

[0044] Injection volume: 10 μL.

[0045] Experimental steps:

[0046] Take an appropriate amount of asenapine maleate and its impurities, dissolve the samples with acetonitrile respectively, and prepare a sample solution containing about 0.5 mg / mL of asenapine maleate and its impurities; another appropriate am...

Embodiment 2

[0048] Instruments and Conditions:

[0049] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0050] Column: C 8 (Apollo, 250×4.6mm, 5μm)

[0051]Mobile phase: Phase A: 0.02mol / L potassium dihydrogen phosphate buffer solution (weigh 2.72g of potassium dihydrogen phosphate, add water to dissolve and set the volume to 1000mL, adjust the pH value to 3.5 with dilute phosphoric acid), phase B: methanol, using a gradient Elution;

[0052] T(min) 0 30 40 60 61 70 B% 40 52 70 75 40 40

[0053] Flow rate: 1.0mL / min

[0054] Detection wavelength: 220nm

[0055] Column temperature: 25°C

[0056] Injection volume: 10 μL.

[0057] Experimental steps:

[0058] Take an appropriate amount of asenapine maleate and its impurities, dissolve the samples in methanol respectively, and prepare a sample solution containing about 0.5 mg / mL of asenapine maleate and its impurities; another appropriate amount of met...

Embodiment 3

[0060] Instruments and Conditions:

[0061] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0062] Column: C 8 (Apollo, 250×4.6mm, 5μm)

[0063] Mobile phase: Phase A: 0.02mol / L potassium dihydrogen phosphate buffer solution (weigh 2.72g of potassium dihydrogen phosphate, add water to dissolve and set the volume to 1000mL, adjust the pH value to 3.5 with dilute phosphoric acid), phase B: methanol, using a gradient Elution;

[0064] T(min) 0 30 40 70 71 80 B% 40 50 50 75 40 40

[0065] Flow rate: 1.0mL / min

[0066] Detection wavelength: 220nm

[0067] Column temperature: 25°C

[0068] Injection volume: 10 μL.

[0069] Experimental steps:

[0070] Take an appropriate amount of asenapine maleate and its impurities, dissolve the samples in methanol respectively, and prepare a sample solution containing about 0.5 mg / mL of asenapine maleate. Perform HPLC analysis according to the above condi...

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PUM

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Abstract

The invention belongs to the field of analytical chemistry and discloses a method for separating and determining maleic acid asenapine and impurities thereof by a liquid chromatography. The method adopts a chromatographic column taking octyl silane bonded silica gel as a filler, buffer salt solution-organic phase with certain proportion is used as a moving phase, the contents of the maleic acid asenapine and the impurities thereof can be quantitatively determined, and the quality of the maleic acid asenapine can be effectively controlled. The method has strong specificity, high accuracy and convenience in operation.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for liquid chromatography separation and determination of asenapine maleate and its impurities. Background technique [0002] Asenapine maleate for acute mania or bipolar disorder with / without psychosis. Asenapine maleate chemical name (3aRS,12bRS) -5-Chloro-2-methyl-2,3,3a,12b-tetrahydro-1 H -dibenzo[2,3:6,7]oxepino[4,5-c]pyrrole(2Z)-2-butenedioate(1:1), the molecular formula is C 21 h 20 ClNO 5 . The structural formula of asenapine maleate is: [0003] [0004] In the process of synthesizing the compound, some important intermediates may be incompletely removed, and degradation impurities may also be produced during the transportation and storage of the compound, and these incompletely removed intermediates and degradation impurities will affect the purity and quality. There are 7 impurities that need to be controlled for asenapine maleate, which are impu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 赵路路刘秋叶王宇杰
Owner AVENTIS PHARMA HAINAN
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