Method for separating and determining related substances of lurasidone hydrochloride intermediate by using gas chromatography

A technology of lurasidone hydrochloride and gas chromatography 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 the problems of affecting the purity and quality of drugs, incomplete removal of impurities and the like , to solve the problem of separation and determination, improve the yield, and reduce the effect of side reactions

Active Publication Date: 2016-08-31
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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  • Method for separating and determining related substances of lurasidone hydrochloride intermediate by using gas chromatography
  • Method for separating and determining related substances of lurasidone hydrochloride intermediate by using gas chromatography
  • Method for separating and determining related substances of lurasidone hydrochloride intermediate by using 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 a...

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 ...

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...

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PUM

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Abstract

The invention discloses a method for separating and determining a lurasidone hydrochloride intermediate (1R,2R)-1,2-cyclohexanedimethanol and related substances thereof by using gas chromatography. The method employs a polysiloxane nonpolar capillary chromatographic column and a hydrogen flame ionization detector, can quantitatively determine the contents of the lurasidone hydrochloride intermediate and the related substances thereof, so purity of reactants in the process of synthesis of lurasidone hydrochloride is effectively controlled, occurrence of side reactions and generation of impurities are reduced, and product yield is improved. The method provided by the invention is fast in separation and detection, good in specificity, high in accuracy, and easy and simple to operate.

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 Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 刘静刘秋叶
Owner BEIJING VENTUREPHARM BIOTECH
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