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A method of separating and measuring optical isomers of a lurasidone intermediate by gas chromatography

A technology of optical isomers and gas chromatography is applied in the field of separation and determination of lurasidone intermediates and optical isomers thereof by gas chromatography, and can solve the problems of incomplete removal of optical impurities, affecting the purity and quality of medicines, and the like, Achieve the effect of ensuring purity and quality

Inactive Publication Date: 2016-04-06
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Incomplete removal of optical impurities in the lurasidone intermediate will be introduced into the final product of the API, thereby affecting the purity and quality of the drug

Method used

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  • A method of separating and measuring optical isomers of a lurasidone intermediate by gas chromatography
  • A method of separating and measuring optical isomers of a lurasidone intermediate by gas chromatography
  • A method of separating and measuring optical isomers of a lurasidone intermediate by gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Instruments and Conditions

[0038] Chromatograph: Agilent6890N gas chromatograph;

[0039] Detector: hydrogen flame ionization detector;

[0040] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.250mm, 0.25μm);

[0041] Column temperature: the initial temperature is 50°C, and the temperature is raised to 170°C at a rate of 20°C per minute, and the temperature is kept constant for 20 minutes;

[0042] Injection port temperature: 200°C;

[0043] Detector temperature: 230°C;

[0044] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0045] Split ratio: 80.0:1;

[0046] Injection volume: 1μL

[0047] Experimental procedure

[0048] Take an appropriate amount of lurasidone intermediate and its optical isomer, dissolve it in dimethyl sulfoxide, and prepare a solution containing 1.0 mg of lurasidone intermediate and 0.1 mg of its optical isomer per 1 mL; another two Methyl sulfoxide was used as a blank solution. Analyze according to the above chromato...

Embodiment 2

[0050] Instruments and Conditions

[0051] Chromatograph: Agilent6890N gas chromatograph;

[0052] Detector: hydrogen flame ionization detector;

[0053] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.250mm, 0.25μm);

[0054] Column temperature: the initial temperature is 50°C, and the temperature is raised to 170°C at a rate of 20°C per minute, and the temperature is kept constant for 20 minutes;

[0055] Injection port temperature: 200°C;

[0056] Detector temperature: 230°C;

[0057] Carrier gas (nitrogen) flow rate: 0.9mL / min;

[0058] Split ratio: 80.0:1;

[0059] Injection volume: 1μL

[0060] Experimental procedure

[0061]Take an appropriate amount of lurasidone intermediate and its optical isomer, dissolve it in dimethyl sulfoxide, and prepare a mixed solution containing 1.0 mg of lurasidone intermediate and 0.1 mg of its optical isomer per 1 mL. Inject the above-mentioned lurasidone intermediate and its optical isomer mixed solution into ...

Embodiment 3

[0063] Instruments and Conditions

[0064] Chromatograph: Agilent6890N gas chromatograph;

[0065] Detector: hydrogen flame ionization detector;

[0066] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.250mm, 0.25μm);

[0067] Column temperature: the initial temperature is 50°C, and the temperature is raised to 170°C at a rate of 20°C per minute, and the temperature is kept constant for 20 minutes;

[0068] Injection port temperature: 195°C;

[0069] Detector temperature: 230°C;

[0070] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0071] Split ratio: 80.0:1;

[0072] Injection volume: 1μL

[0073] Experimental procedure

[0074] Take an appropriate amount of lurasidone intermediate and its optical isomer, dissolve it in dimethyl sulfoxide, and prepare a mixed solution containing 1.0 mg of lurasidone intermediate and 0.1 mg of its optical isomer per 1 mL. Inject the above-mentioned lurasidone intermediate and its optical isomer mixed solution into...

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PUM

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method of measuring optical purity of a lurasidone intermediate that is (1R,2R)-1,2-cyclohexanedimethanol by gas chromatography. The method adopts a cyclodextrin type chiral capillary chromatographic column and a flame ionization detector, can quantificationally measure the optical purity and contents of isomers of the lurasidone intermediate, and can indicate stability of the optical isomers of the lurasidone intermediate. The method is high in specificity, high in accuracy and simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring lurasidone intermediates and optical isomers thereof by gas chromatography. Background technique [0002] Lurasidone is an atypical antipsychotic drug clinically used in the treatment of schizophrenia to improve cognitive function. The chemical name of lurasidone is (3aR, 4S, 7R, 7aS)-2-﹛(1R, 2R)-2-[4-(1,2-benzisothiazol-3-yl)piperazin-1-ylmethyl]cyclohexylmethyl﹜ hexahydro-4,7-methano-2H-isoindole-1,3-dione, molecular formula C 28 h 36 N 4 o 2 S. Lurasidone intermediate chemical name (1R,2R)-1,2-Cyclohexanedimethanol, molecular formula is C 8 h 16 o 2 , the structural formula is: [0003] [0004] In the process of drug development, it is particularly important to establish chiral analysis methods for raw materials and key intermediates. Lurasidone has a chiral center and is an optically active compound. In order ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 齐连静刘秋叶
Owner BEIJING VENTUREPHARM BIOTECH
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