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A method for separating and determining lurasidone hydrochloride intermediate related substances by gas chromatography

A technology of lurasidone hydrochloride and gas chromatography, which is applied in the field of separation and determination of the chemical purity of lurasidone hydrochloride intermediates and related substances by gas chromatography, and can solve problems affecting the purity and quality of drugs and incomplete removal of impurities , to achieve the effect of solving the problem of separation and determination, increasing the yield and reducing side reactions

Active Publication Date: 2022-02-11
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Incomplete removal of impurities in lurasidone hydrochloride intermediate will affect the purity and quality of the drug

Method used

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  • A method for separating and determining lurasidone hydrochloride intermediate related substances by gas chromatography
  • A method for separating and determining lurasidone hydrochloride intermediate related substances by gas chromatography
  • A method for separating and determining lurasidone hydrochloride intermediate related substances by gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Instruments and Conditions

[0039] Chromatograph: Agilent 7890A gas chromatograph;

[0040] Detector: hydrogen flame ionization detector;

[0041] Chromatographic column: DB-1 capillary column (Agilent, 30m´0.53mm´1.5mm);

[0042] Injection port temperature: 250°C;

[0043] Detector temperature: 300°C;

[0044] Carrier gas (nitrogen) flow rate: 2.5mL / min;

[0045] Split ratio: 20:1;

[0046] Injection volume: 1μL

[0047] Oven heating program:

[0048] Heating rate (℃ / min) temperature (°C) Hold time (min) / 150 5 10 220 3

[0049] Experimental procedure

[0050] Take an appropriate amount of lurasidone hydrochloride intermediate and its related substances, dissolve them in dimethyl sulfoxide, and prepare a solution containing 0.1-10 mg of each 1 mL of lurasidone hydrochloride intermediate and its related substances; Sulfoxide was used as a blank solution. Analyze according to the above chromatographic conditions and record the chr...

Embodiment 2

[0052] Instruments and Conditions

[0053] Chromatograph: Agilent 7890A gas chromatograph;

[0054] Detector: hydrogen flame ionization detector;

[0055] Chromatographic column: DB-1 capillary column (Agilent, 30m´0.53mm´1.5mm);

[0056] Injection port temperature: 250°C;

[0057] Detector temperature: 300°C;

[0058] Carrier gas (nitrogen) flow rate: 2.4mL / min;

[0059] Split ratio: 20:1;

[0060] Injection volume: 1μL

[0061] Oven heating program:

[0062] Heating rate (℃ / min) temperature (°C) Hold time (min) / 150 5 10 220 3

[0063] Experimental procedure

[0064] Take an appropriate amount of lurasidone hydrochloride intermediate and its related substances, dissolve them in dimethyl sulfoxide, and prepare a mixed solution containing 0.1-10 mg of each 1 mL of lurasidone hydrochloride intermediate and its related substances; sulfoxide as a blank solution. The above-mentioned lurasidone hydrochloride intermediate and its related subst...

Embodiment 3

[0066] Instruments and Conditions

[0067] Chromatograph: Agilent 7890A gas chromatograph;

[0068] Detector: hydrogen flame ionization detector;

[0069] Chromatographic column: DB-1 capillary column (Agilent, 30m´0.53mm´1.5mm);

[0070] Injection port temperature: 240°C;

[0071] Detector temperature: 300°C;

[0072] Carrier gas (nitrogen) flow rate: 2.5mL / min;

[0073] Split ratio: 20:1;

[0074] Injection volume: 1μL

[0075] Oven heating program:

[0076] Heating rate (℃ / min) temperature (°C) Hold time (min) / 150 5 10 220 3

[0077] Experimental procedure

[0078] Take an appropriate amount of lurasidone hydrochloride intermediate and its related substances, dissolve them in dimethyl sulfoxide, and prepare a mixed solution containing 0.1-10 mg of each 1 mL of lurasidone hydrochloride intermediate and its related substances; sulfoxide as blank solvent. The above-mentioned lurasidone hydrochloride intermediate and its related substanc...

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Abstract

The invention belongs to the field of analytical chemistry, and the invention discloses a method for separating and detecting lurasidone hydrochloride intermediate (1R,2R)-1,2-cyclohexanedimethanol and its related substances by gas chromatography. Using polysiloxane non-polar capillary chromatographic column and hydrogen flame ionization detector, the content of lurasidone hydrochloride intermediate and related substances can be quantitatively determined, so as to effectively control the reactants in the process of synthesizing lurasidone hydrochloride The purity of the product can reduce the occurrence of side reactions and the generation of impurities, and improve the product yield. The method of the invention has fast separation and detection, strong specificity, high accuracy and simple operation.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring the chemical purity of lurasidone hydrochloride intermediates and related substances by gas chromatography. Background technique [0002] Lurasidone hydrochloride is an atypical antipsychotic drug clinically used in the treatment of schizophrenia to improve cognitive function. The chemical name of lurasidone hydrochloride is (3aR,4S,7R,7aS)-2-{(1R,2R)-2-[4-(1,2-benzisothiazol-3-yl)piperazine-1 -Methylene]cyclohexylmethyl}hexahydro-4,7-endomethylene-2H-isoindole-1,3-dione hydrochloride, the molecular formula is C 28 h 36 N 4 o 2 S HCl. The chemical name of lurasidone hydrochloride intermediate is (1R,2R)-1,2-cyclohexanedimethanol, and the molecular formula is C 8 h 16 o 2 , the structural formula is: [0003] [0004] In the process of synthesizing lurasidone hydrochloride, it is necessary to control the purity of some important...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 刘静刘秋叶
Owner BEIJING VENTUREPHARM BIOTECH
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