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Accurate quantitative determination method for impurity homopiperazine in medicine

A quantitative determination, high piperazine technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of cumbersome operation and low accuracy, and achieve the effect of high measurement efficiency, improved accuracy, and good measurement accuracy.

Active Publication Date: 2021-05-04
上海微谱检测科技集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of low accuracy and cumbersome operation of the method for determining the content of homopiperazine in the existing fasudil hydrochloride injection, the first aspect of the present invention provides an accurate quantitative determination method for homopiperazine in the fasudil hydrochloride injection, It has the advantages of short detection time, high sensitivity, good accuracy and good repeatability

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  • Accurate quantitative determination method for impurity homopiperazine in medicine
  • Accurate quantitative determination method for impurity homopiperazine in medicine
  • Accurate quantitative determination method for impurity homopiperazine in medicine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] This example provides an accurate quantitative determination of homopiperazine, including:

[0083] (1) Sample solution preparation: Take the drug in a 20ml brown sample bottle, add 10.00ml of diluent, mix well, then add 10.00ml of organic solvent, and finally add chlorine salt until the bottom appears like quicksand, vortex for 0.5 minutes, and let stand for 5 Minutes, get about 1ml of upper layer solution in 2ml brown sampling vial, as sample solution; Described diluent is the sodium hydroxide aqueous solution of 0.1mol / L, and described organic solvent is acetonitrile, and described chlorate is sodium chloride;

[0084] (2) Determination: measure the content of homopiperazine in the sample solution with ultra-high performance liquid chromatography-tandem mass spectrometry;

[0085] The condition of described ultra-high performance liquid chromatography is:

[0086] Chromatographic column: ACQUITY UPLC BEH C18, 2.1mm×50mm, 1.7μm;

[0087] Flow rate: 0.19mL / min;

[0...

Embodiment 2

[0102] This example provides an accurate quantitative determination of homopiperazine, including:

[0103] (1) Sample solution preparation: Take the drug in a 20ml brown sample bottle, add 10.00ml of diluent, mix well, then add 10.00ml of organic solvent, and finally add chlorine salt until the bottom appears like quicksand, vortex for 0.5 minutes, and let stand for 5 Minutes, get about 1ml of upper layer solution in the 2ml brown sampling vial, as sample solution; Described diluent is the sodium hydroxide aqueous solution of 5mol / L, and described organic solvent is acetonitrile, and described chlorate is sodium chloride;

[0104] (2) Determination: measure the content of homopiperazine in the sample solution with ultra-high performance liquid chromatography-tandem mass spectrometry;

[0105] The condition of described ultra-high performance liquid chromatography is:

[0106] Chromatographic column: ACQUITY UPLC BEH C18, 2.1mm×50mm, 1.7μm;

[0107] Flow rate: 0.21mL / min;

...

Embodiment 3

[0122] This example provides an accurate quantitative determination of homopiperazine, including:

[0123] (1) Sample solution preparation: Take the drug in a 20ml brown sample bottle, add 10.00ml of diluent, mix well, then add 10.00ml of organic solvent, and finally add chlorine salt until the bottom appears like quicksand, vortex for 0.5 minutes, and let stand for 5 Minutes, get about 1ml of upper layer solution in 2ml brown sampling vial, as sample solution; Described diluent is the sodium hydroxide aqueous solution of 1mol / L, and described organic solvent is acetonitrile, and described chlorate is sodium chloride;

[0124] (2) Determination: measure the content of homopiperazine in the sample solution with ultra-high performance liquid chromatography-tandem mass spectrometry;

[0125] The condition of described ultra-high performance liquid chromatography is:

[0126] Chromatographic column: ACQUITY UPLC BEH C18, 2.1mm×50mm, 1.7μm;

[0127] Flow rate: 0.2mL / min;

[0128...

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Abstract

The invention relates to determination of homopiperazine, in particular to an accurate quantitative determination method for impurity homopiperazine in a medicine. The method comprises the following steps of: (1) preparation of a sample solution: sequentially adding a diluent and an organic solvent into the medicine, and performing mixing to obtain the sample solution; and (2) determination. The invention provides an accurate quantitative determination method of homopiperazine, and the method can be used for determination of homopiperazine in fasudil hydrochloride medicines. An accurate quantitative determination result can be obtained through an ultrahigh liquid chromatography-tandem mass spectrometry mode, and the method has high determination efficiency; by designing the preparation method of the sample solution, the alkaline diluent and the organic solvent are selected to dilute the medicine, and the obtained sample solution has high accuracy and recovery rate when being used for determination; a chlorine salt is added into the sample solution, so that the high accuracy and the recovery rate can be promoted, and the long-time stability of the sample solution can be improved.

Description

technical field [0001] The invention relates to the determination of homopiperazine, more specifically, the invention relates to an accurate quantitative determination method of homopiperazine as an impurity in medicine. Background technique [0002] Fasudil hydrochloride is a new type of drug with a wide range of pharmacological effects. Its molecular structure is a 5-isoquinoline sulfonamide derivative, which is an RHO kinase inhibitor and expands blood vessels by increasing the activity of myosin light chain phosphatase , reduce the tension of endothelial cells, improve the microcirculation of brain tissue, prevent and aggravate cerebral blood stealing, and at the same time antagonize inflammatory factors, protect nerves against apoptosis, and promote nerve regeneration. The results show that fasudil hydrochloride has a certain effect on promoting the recovery of nerve function, relieving clinical symptoms and reducing the disability rate. Therefore, due to the constrain...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/34G01N30/72
Inventor 汪辉秦秋明邵红霞刘婷
Owner 上海微谱检测科技集团股份有限公司