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

A technology for lurasidone hydrochloride and related substances, which is applied in the field of separation and determination of lurasidone hydrochloride intermediates and related substances by gas chromatography technology, can solve the problems of incomplete removal of impurities and influence on the purity and quality of drugs, and achieve separation and determination problems, increase yield, and reduce the effect of side reactions

Active Publication Date: 2022-07-22
BEIJING VENTUREPHARM BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Incomplete removal of impurities in the lurasidone hydrochloride intermediate will affect the purity and quality of the final 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

[0034] Instruments and Conditions

[0035] Chromatograph: Agilent 7890A gas chromatograph;

[0036] Detector: hydrogen flame ionization detector;

[0037] Chromatographic column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0038] Inlet temperature: 180℃;

[0039] Detector temperature: 250℃;

[0040] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0041] Split ratio: 10:1;

[0042] Injection volume: 1 μL.

[0043] Oven temperature program:

[0044] Heating rate (℃ / min) Temperature (℃) Hold time (min) / 50 5 10 180 7

[0045] Experimental steps:

[0046] Take an appropriate amount of lurasidone hydrochloride, dissolve it in dimethyl sulfoxide to make a solution containing 100 mg lurasidone hydrochloride per 1ml, as the test solution; take an appropriate amount of piperazine, n-butanol and ethyl acetate, add two Methyl sulfoxide was dissolved to prepare a solution containing about 0.5 mg each of piperazine, n-butanol and ethyl ace...

Embodiment 2

[0048] Instruments and Conditions

[0049] Chromatograph: Agilent 7890A gas chromatograph;

[0050] Detector: hydrogen flame ionization detector;

[0051] Chromatographic column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0052] Inlet temperature: 190℃;

[0053] Detector temperature: 250℃;

[0054] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0055] Split ratio: 10:1;

[0056] Injection volume: 1 μL

[0057] Oven temperature program:

[0058] Heating rate (℃ / min) Temperature (℃) Hold time (min) / 50 5 10 180 7

[0059] Experimental steps:

[0060] Take an appropriate amount of piperazine, n-butanol and ethyl acetate, add dimethyl sulfoxide and dissolve it to prepare a solution containing about 0.5 mg each of piperazine, n-butanol and ethyl acetate per 1 ml, as the test solution; Methyl sulfoxide was used as blank solution. The above-mentioned test solution and blank solution were injected into the gas chromatograph, analyz...

Embodiment 3

[0062] Instruments and Conditions

[0063] Chromatograph: Agilent 7890A gas chromatograph;

[0064] Detector: hydrogen flame ionization detector;

[0065] Chromatographic column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0066] Inlet temperature: 180℃;

[0067] Detector temperature: 250℃;

[0068] Carrier gas (nitrogen) flow rate: 1.1mL / min;

[0069] Split ratio: 10:1;

[0070] Injection volume: 1 μL.

[0071] Oven temperature program:

[0072] Heating rate (℃ / min) Temperature (℃) Hold time (min) / 50 5 10 180 7

[0073] Experimental steps:

[0074] Take an appropriate amount of piperazine, n-butanol and ethyl acetate, add dimethyl sulfoxide and dissolve it to prepare a solution containing about 0.5 mg each of piperazine, n-butanol and ethyl acetate per 1 ml, as the test solution; Methyl sulfoxide was used as blank solution. The above-mentioned test solution and blank solution were injected into the gas chromatograph, analy...

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for separating and detecting related substances of lurasidone hydrochloride intermediate 3-(1-piperazinyl)-1,2-benzisothiazole by gas chromatography technology. Siloxane type medium polar capillary chromatographic column, hydrogen flame ionization detector, can quantitatively determine the content of lurasidone hydrochloride intermediate related substances, so as to effectively control the purity of the reactants in the process of synthesizing lurasidone hydrochloride, reduce The occurrence of side reactions and the generation of impurities improve the product yield. The method of the invention has the advantages of rapid 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 lurasidone hydrochloride intermediate related substances by gas chromatography. Background technique [0002] Lurasidone hydrochloride is a new type of antipsychotic drug with dual action. It has high affinity for both 5-HT2A receptors and dopamine D2 receptors, and has significant curative effect on both positive and negative symptoms of psychotic patients. 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-methylene-2H-isoindole-1,3-dione hydrochloride, the molecular formula is C 28 H 36 N 4 O 2 S·HCl. Lurasidone hydrochloride intermediate chemical name 3-(1-piperazinyl)-1,2-benzisothiazole, molecular formula is C 11 H 13 N 3 S, the structural formula is: [0003] [0004] In the process of synthesizing lurasidone hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 孙冬雪王宇杰
Owner BEIJING VENTUREPHARM BIOTECH
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