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Method for detecting dimethylamine contained in sarpogrelate hydrochloride intermediate

A technology of sagrelate hydrochloride and detection method, which is applied in the field of detection of dimethylamine in intermediates containing sarcogrelate hydrochloride, can solve the problem of residual, sarcogrelate hydrochloride raw material drug quality impact, and dimethylamine-free detection method research disclosure And other issues

Inactive Publication Date: 2018-06-29
TIANJIN CHASE SUN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the above route, dimethylamine is one of the reaction raw materials of intermediate C, and simultaneously dimethylamine and hydrochloric acid participate in the reaction, which inevitably produces dimethylamine hydrochloride. residues, and will participate in the follow-up reaction at the same time, which will affect the quality of sargrelate hydrochloride API
[0009] At present, there is no published research on the detection method of dimethylamine in intermediate C

Method used

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  • Method for detecting dimethylamine contained in sarpogrelate hydrochloride intermediate
  • Method for detecting dimethylamine contained in sarpogrelate hydrochloride intermediate
  • Method for detecting dimethylamine contained in sarpogrelate hydrochloride intermediate

Examples

Experimental program
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Effect test

Embodiment 1

[0150] The detection of dimethylamine and dimethylamine hydrochloride in embodiment 1 intermediate C

[0151] The test solution: Accurately weigh about 0.1g of intermediate C, put it in a 10ml headspace bottle, add 1ml of dimethyl sulfoxide, 0.5ml of 8mol / L potassium hydroxide, and seal it with a gland, as the test solution.

[0152] Accurately weigh an appropriate amount of dimethylamine reference substance, add dimethyl sulfoxide to make a solution containing about 0.1mg of dimethylamine per 1ml, accurately measure 1ml, put it in a 10ml headspace bottle, add 8mol / L potassium hydroxide 0.5 ml, sealed with a gland, as a reference solution.

[0153] Chromatographic conditions:

[0154] Chromatographic column: use InertCap for Amines, (0.32mm×30mm) or similar polarity chromatographic column as the chromatographic column;

[0155] Heating program:

[0156] The temperature program was raised to an initial temperature of 40°C, raised to 90°C at a rate of 10°C / min, then raised to...

Embodiment 2

[0167] The detection of dimethylamine and dimethylamine hydrochloride in the intermediate C of embodiment 2

[0168] The test solution: Accurately weigh about 0.1g of intermediate C, put it in a 10ml headspace bottle, add 1ml of dimethyl sulfoxide, 0.5ml of 8mol / L potassium hydroxide, and seal it with a gland, as the test solution.

[0169] Accurately weigh an appropriate amount of dimethylamine reference substance, add dimethyl sulfoxide to make a solution containing about 0.1mg of dimethylamine per 1ml, accurately measure 1ml, put it in a 10ml headspace bottle, add 8mol / L potassium hydroxide 0.5 ml, sealed with a gland, as a reference solution.

[0170] Chromatographic conditions:

[0171] Chromatographic column: use InertCap for Amines, (0.32mm×30mm) or similar polarity chromatographic column as the chromatographic column;

[0172] Heating program:

[0173] The temperature program was raised to an initial temperature of 35°C, raised to 90°C at a rate of 10°C / min, then ra...

Embodiment 3

[0184] The detection of dimethylamine and dimethylamine hydrochloride in the intermediate C of embodiment 3

[0185] The test solution: Accurately weigh about 0.1g of intermediate C, put it in a 10ml headspace bottle, add 1ml of dimethyl sulfoxide, 0.5ml of 8mol / L potassium hydroxide, and seal it with a gland, as the test solution.

[0186] Accurately weigh an appropriate amount of dimethylamine reference substance, add dimethyl sulfoxide to make a solution containing about 0.1mg of dimethylamine per 1ml, accurately measure 1ml, put it in a 10ml headspace bottle, add 8mol / L potassium hydroxide 0.5 ml, sealed with a gland, as a reference solution.

[0187] Chromatographic conditions:

[0188] Chromatographic column: use InertCap for Amines, (0.32mm×30mm) or similar polarity chromatographic column as the chromatographic column;

[0189] Heating program:

[0190] The temperature program was raised to an initial temperature of 45°C, raised to 90°C at a rate of 10°C / min, then ra...

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Abstract

The invention discloses a method for detecting dimethylamine and dimethylamine hydrochloride in a sarpogrelate hydrochloride intermediate C. The method is simple, and favorable in precision, accuracy,reproducibility and durability. The method can be used for detecting the dimethylamine and the dimethylamine hydrochloride in the sarpogrelate hydrochloride intermediate C, i.e. 1-(dimethylamino)-3-[2-[2-(3-methoxyphenyl) ethyl] phenoxy]-2-propanol hydrochloride.

Description

technical field [0001] The invention belongs to the field of drug detection, and in particular relates to a method for detecting dimethylamine contained in a sagrelate hydrochloride intermediate. Background technique [0002] Sarpogrelate hydrochloride is a 5-hydroxytryptamine (5-HT2) receptor blocker that can specifically bind to 5-HT2 receptors. 5-hydroxytryptamine (5-HT) was first proposed as a vasoactive substance in 1955. 5-HT exists widely in animals, especially in the cardiovascular system. Except for a small part that is re-uptaked and stored in platelets, almost all 5-HT is inactivated by endothelial cells in the liver and lungs. Sagrelate hydrochloride can specifically bind to 5-HT2 receptors, showing a special antagonistic effect on receptors on platelets and vascular smooth muscle. Therefore, it exhibits anti-platelet effect and inhibits vasoconstriction, and exerts a series of biological effects. Sagrelate hydrochloride is an antithrombotic drug, mainly used ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 韩冬许磊贺英郭嘉林孔凯刘登科董凯
Owner TIANJIN CHASE SUN PHARM CO LTD
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