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High performance liquid phase detection method of homopiperazine

A high-performance liquid phase and detection method technology, applied in the field of liquid chromatography detection, can solve the problems of low accuracy, cumbersome operation, difficult to control, etc., and achieve the effects of high precision, good reproducibility and good stability

Active Publication Date: 2019-12-20
SHANDONG WEIGAO PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has weak retention on conventional reversed-phase chromatographic columns, and has no UV absorption, and is not suitable for gas phase detection after salt formation, so it is not easy to control in production. Since homopiperazine has no UV absorption and high polarity, it is highly efficient Liquid chromatography cannot be used for effective detection. It has been reported in the literature that the content of homopiperazine in fasudil hydrochloride has been determined by liquid chromatography, ultraviolet spectrophotometry, and ion chromatography, but the existing detection methods have low accuracy in determining the structure , cumbersome operation

Method used

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  • High performance liquid phase detection method of homopiperazine
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  • High performance liquid phase detection method of homopiperazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Chromatographic conditions use octadecylsilane bonded silica gel as filler; use 0.02mol / L sodium acetate trihydrate (pH=5.0)-acetonitrile (75:25) as mobile phase to adopt gradient elution; detection wavelength is 248nm, column The temperature was 30°C, and the injection volume was 10 μl.

[0049] Determination method: Precisely measure the appropriate amount of this product and homopiperazine reference substance, add water to dissolve and quantitatively dilute to make a solution containing about 0.6mg of fasudil hydrochloride and 0.6μg of homopiperazine in every 1ml, as the test solution; Another appropriate amount of homopiperazine reference substance was taken, accurately weighed, dissolved in water and quantitatively diluted to make a solution containing about 1.2 μg of homopiperazine per 1 ml, as the reference substance solution.

[0050] Sample derivation: Accurately measure 10 μl of the test solution, place it in a dry derivation tube with a diameter of 6 mm and a...

Embodiment 2

[0052] Chromatographic conditions: use octadecylsilane bonded silica gel as filler; use 0.02mol / L sodium acetate trihydrate (pH=5.0)-acetonitrile (78:22) as mobile phase, use isocratic elution; detection wavelength is 248nm, column temperature 30°C, injection volume 10μl.

[0053] Determination method: Precisely measure the appropriate amount of this product and homopiperazine reference substance, add water to dissolve and quantitatively dilute to make a solution containing about 0.6mg of fasudil hydrochloride and 0.6μg of homopiperazine in every 1ml, as the test solution; Another appropriate amount of homopiperazine reference substance was taken, accurately weighed, dissolved in water and quantitatively diluted to make a solution containing about 1.2 μg of homopiperazine per 1 ml, as the reference substance solution.

[0054]Sample derivation: Accurately measure 10 μl of the test solution, place it in a dry derivation tube with a diameter of 6 mm and a height of 50 mm, add 70...

Embodiment 3

[0056] Chromatographic conditions: use octadecylsilane bonded silica gel as filler; use 0.02mol / L sodium acetate trihydrate (pH=5.0)-acetonitrile (72:28) as mobile phase, use isocratic elution; 1.0ml per minute, the detection wavelength is 248nm, the column temperature is 30°C, and the injection volume is 10μl.

[0057] Determination method: Precisely measure the appropriate amount of this product and homopiperazine reference substance, add water to dissolve and quantitatively dilute to make a solution containing about 0.6mg of fasudil hydrochloride and 0.6μg of homopiperazine in every 1ml, as the test solution; Another appropriate amount of homopiperazine reference substance was taken, accurately weighed, dissolved in water and quantitatively diluted to make a solution containing about 1.2 μg of homopiperazine per 1 ml, as the reference substance solution.

[0058] Sample derivation: Accurately measure 10 μl of the test solution, place it in a dry derivation tube with a diame...

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Abstract

The invention discloses a high performance liquid phase detection method of homopiperazine. The high performance liquid phase detection method comprises the steps of: diluting a fasudil hydrochlorideinjection with water and adding homopiperazine into the diluted fasudil hydrochloride injection; adding a borate buffered saline and a derivatization reagent into a dry derivatization tube; sealing the derivatization tube with a paraffin film, heating the derivatization tube, and cooling the derivatization tube to obtain a derivative sample; and acquiring a chromatogram of the derivative sample byadopting a liquid chromatograph, and measuring the content of homopiperazine. On the basis of a reversed-phase high-performance liquid phase chromatographic pre-column derivatization method-AccQ.Tagmethod developed by the Waters company, the derivatization reagent is used for adding a fluorophore onto an amino group of homopiperazine; the modified homopiperazine derivative has ultraviolet absorption, and qualitative and quantitative analysis is carried out by using high performance liquid phase chromatography. The high performance liquid phase detection method disclosed by the invention is high in precision, good in stability and good in reproducibility, enriches the method for detecting the homopiperazine content, and fills the blank that only ion chromatography can be used for liquid phase detection of the homopiperazine content.

Description

technical field [0001] The invention relates to the field of liquid chromatography detection, in particular to a high-efficiency liquid phase detection method with high piperazine content. Background technique [0002] Fasudil hydrochloride is a myosin light chain phosphorylase, RHO kinase inhibitor and a new type of intracellular calcium ion anticoagulation agent. The drug can improve the microcirculation of brain tissue, effectively relieve cerebral vasospasm, and protect ischemia Brain tissue, promoting nerve regeneration, is a new type of drug with a wide range of pharmacological effects, and homopiperazine is an intermediate in the synthesis of fasudil hydrochloride. It has weak retention on conventional reversed-phase chromatographic columns, and has no UV absorption, and is not suitable for gas phase detection after salt formation, so it is not easy to control in production. Since homopiperazine has no UV absorption and high polarity, it is highly efficient Liquid ch...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06G01N30/89
CPCG01N30/06G01N30/88G01N30/89G01N2030/067G01N2030/884
Inventor 杨万运王智军肖海荣孙国琳潘潇
Owner SHANDONG WEIGAO PHARM CO LTD
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