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Method for separating and measuring relevant substance of lurasidone hydrochloride intermediate by using gas chromatographic technique

A technology of lurasidone hydrochloride and gas chromatography, which is applied in the field of separation and determination of lurasidone hydrochloride intermediate related substances by gas chromatography technology, can solve the problems of affecting the purity and quality of medicine, incomplete removal of impurities, etc., and achieves separation and determination problems, improving yield, reducing the effect of side reactions

Active Publication Date: 2017-03-22
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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  • Method for separating and measuring relevant substance of lurasidone hydrochloride intermediate by using gas chromatographic technique
  • Method for separating and measuring relevant substance of lurasidone hydrochloride intermediate by using gas chromatographic technique
  • Method for separating and measuring relevant substance of lurasidone hydrochloride intermediate by using gas chromatographic technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Apparatus and conditions

[0037] Chromatograph: Agilent 7890A gas chromatograph;

[0038] Detector: hydrogen flame ionization detector;

[0039] Column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0040] Inlet temperature: 180℃;

[0041] Detector temperature: 250℃;

[0042] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0043] Split ratio: 10:1;

[0044] Injection volume: 1μL.

[0045] Oven heating program:

[0046] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 505 101807

[0047] Experimental steps:

[0048] Take an appropriate amount of lurasidone hydrochloride and add dimethyl sulfoxide to make a solution containing 100mg of lurasidone hydrochloride per 1ml, as the test solution; take appropriate amount of piperazine, n-butanol and ethyl acetate, add two Methyl sulfoxide was dissolved to make a solution containing piperazine, n-butanol and ethyl acetate each about 0.5 mg per 1 ml as a reference solution; another dimethyl sulfoxide was taken as a blank so...

Embodiment 2

[0050] Apparatus and conditions

[0051] Chromatograph: Agilent 7890A gas chromatograph;

[0052] Detector: hydrogen flame ionization detector;

[0053] Column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0054] Inlet temperature: 190℃;

[0055] Detector temperature: 250℃;

[0056] Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0057] Split ratio: 10:1;

[0058] Injection volume: 1μL

[0059] Oven heating program:

[0060] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 505 101807

[0061] Experimental steps:

[0062] Take appropriate amount of piperazine, n-butanol and ethyl acetate, add dimethyl sulfoxide to dissolve to make a solution containing piperazine, n-butanol and ethyl acetate each about 0.5mg per 1ml, as the test solution; take another two Methyl sulfoxide was used as a blank solution. Inject the above-mentioned test solution and blank solution into the gas chromatograph respectively, analyze according to the above-mentioned chromatographic conditions, a...

Embodiment 3

[0064] Apparatus and conditions

[0065] Chromatograph: Agilent 7890A gas chromatograph;

[0066] Detector: hydrogen flame ionization detector;

[0067] Column: DB-624 capillary column (Agilent, 30m´0.32mm, 1.8mm);

[0068] Inlet temperature: 180℃;

[0069] Detector temperature: 250℃;

[0070] Carrier gas (nitrogen) flow rate: 1.1mL / min;

[0071] Split ratio: 10:1;

[0072] Injection volume: 1μL.

[0073] Oven heating program:

[0074] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 505 101807

[0075] Experimental steps:

[0076] Take appropriate amount of piperazine, n-butanol and ethyl acetate, add dimethyl sulfoxide to dissolve to make a solution containing piperazine, n-butanol and ethyl acetate each about 0.5mg per 1ml, as the test solution; take another two Methyl sulfoxide was used as a blank solution. Inject the above-mentioned test solution and blank solution into the gas chromatograph respectively, analyze according to the above-mentioned chromatographic conditions, ...

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Abstract

The invention belongs to the field of analytical chemistry, and the invention discloses a method for separating and detecting a relevant substance of a lurasidone hydrochloride intermediate 3-(1-piperazinyl)-1,2-benzisothiazole by using a gas chromatographic technique. A methylpolysilicone medium polar capillary chromatographic column and a hydrogen flame ionization detector are adopted by the method; the content of the relevant substance of the lurasidone hydrochloride intermediate can be quantitatively measured; thus, the purity of a reactant in the process of synthesizing the lurasidone hydrochloride is effectively controlled; the occurrences of side reactions and the generation of impurities are reduced; the yield of a product is improved. The method provided by the invention is quick in separation and detection, high in specificity and high in accuracy, and is simple and convenient to operate.

Description

Technical field [0001] The invention belongs to the field of analytical chemistry, and specifically relates to a method for separating and determining related substances of lurasidone hydrochloride intermediates by gas chromatography technology. Background technique [0002] Lurasidone hydrochloride is a new type of antipsychotic drug with dual effects. It has a high affinity for both 5-HT2A receptor and dopamine D2 receptor, and has significant effects on both the positive and negative symptoms of mental 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 C 11 H 13 N 3 S, the structural formula is: [0003] [0004] In the process of synthesizing lurasidon...

Claims

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Application Information

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