Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride

A technology of ethyl isoquinolinesulfonate and fasudil hydrochloride, which is applied in the field of detection of ethyl 5-isoquinolinesulfonate in fasudil hydrochloride, can solve the problem of 5-isoquinolinesulfonate Ethyl acetate detection method, ineffective detection, long running time and other problems, to achieve the effect of high detection sensitivity, good for safety control, and short running time

Active Publication Date: 2019-02-22
KPC PHARM INC
View PDF6 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The quantitative concentration of this method is 0.337 μg / ml, and the detection limit concentration is 0.084 μg / ml, which is still high, and the sensitivity is not enough, and it cannot effectively detect methyl 5-isoquinolinesulfonate at the ppm level in fasudil hydrochloride
This method is not for the detection of ethyl 5-isoquinolinesulfonate, and the running time is long and the sensitivity is not enough
Also do not see the report about the detection method of ethyl 5-isoquinolinesulfonate in the prior art

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride
  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride
  • Method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]1. Instruments and materials

[0043] 1. Main instruments

[0044] Mass spectrometer: AB SCIEX company, model API 4000.

[0045] Liquid chromatograph: Shimadzu company, model LC20AD.

[0046] Electronic balance: METTLER company, XP205 type.

[0047] 2. Experimental materials

[0048] Ethyl 5-isoquinolinesulfonate reference substance: provided by Kunming Pharmaceutical Group Co., Ltd., with a purity of 97.62%.

[0049] Fasudil hydrochloride API: Kunming Pharmaceutical Group Co., Ltd., batch number 201201-01.

[0050] 2. Experimental method

[0051] 1. Solution preparation

[0052] 1.1 0.1% formic acid-water solution: precisely pipette 1ml of formic acid into 1000ml of water, and mix well.

[0053] 1.2 Diluent: Measure 300ml of water and 700ml of acetonitrile, mix well.

[0054] 1.3 Reference substance stock solution (50ng / ml): Take about 2mg of 5-isoquinolinesulfonate reference substance, accurately weigh it, put it in a 200ml measuring bottle, dissolve it with di...

Embodiment 2

[0100] Embodiment 2, adopt the inventive method to carry out quality analysis to Fasudil hydrochloride

[0101] Fasudil hydrochloride raw material is from Kunming Pharmaceutical Group Co., Ltd., with 3 batches in total, and the batch numbers are 201201-01, 201201-02, and 201201-03.

[0102] The preparation of need testing solution (0.5mg / ml): get fasudil hydrochloride crude drug 10mg, accurately weighed, put in 20ml measuring bottle, dissolve and dilute to scale with diluent, shake up, as need testing solution .

[0103] Get the above-mentioned need testing solution and inject high performance liquid chromatography and use triple quadrupole mass spectrometer in conjunction, record chromatogram (the collection of illustrative plates of 201201-01 batch sees Figure 4 , the spectrum of batch 201201-02 and Figure 4 Similar, for the spectrum of batch 201201-03 see Figure 5 ), calculate the content of genotoxic impurity ethyl 5-isoquinolinesulfonate in the test product accordin...

Embodiment 3

[0108] This embodiment is with embodiment 1, and difference is that the concentration of fasudil hydrochloride need testing solution is 0.4mg / ml, and the concentration of ethyl 5-isoquinolinesulfonate reference substance solution is 0.1ng / ml.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Lengthaaaaaaaaaa
The inside diameter ofaaaaaaaaaa
Particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the field of medicinal chemistry analysis and particularly relates to a method for detecting 5-Isoquinolinesulfonic acid in fasudil hydrochloride. The method is that a high-performance liquid chromatography-mass spectrum system is adopted to detect a 5-Isoquinolinesulfonic acid reference substance solution and a fasudil hydrochloride test sample solution. According to thedetecting method, the high performance liquid chromatography is firstly adopted for component separation, the position of a chromatographic peak of the 5-Isoquinolinesulfonic acid in the fasudil hydrochloride test sample solution can be determined under the chromatographic condition, the chromatographic peak of the 5-Isoquinolinesulfonic acid is effectively separated from chromatographic peak of adjacent other components, and the operation time is short; then, the mass spectrum condition is adopted to quantify a ternary quadrupole rod mass spectrum, ppm level of 5-Isoquinolinesulfonic acid canbe detected, and the limit of quantitation can reach ng / ml. Therefore, the 5-Isoquinolinesulfonic acid in fasudil hydrochloride can be effectively controlled.

Description

technical field [0001] The invention belongs to the field of pharmaceutical chemical analysis, in particular to a method for detecting ethyl 5-isoquinolinesulfonate in fasudil hydrochloride. Background technique [0002] Fasudil hydrochloride is a new type of isoquinoline sulfonamide derivatives, which can dilate blood vessels by increasing the activity of myosin light chain phosphatase, reduce the tension of endothelial cells, improve the microcirculation of brain tissue, and protect ischemic brain tissue. At the same time, it can antagonize inflammatory factors, protect nerves against apoptosis, and promote nerve regeneration. Fasudil hydrochloride and its injection were launched in China in 2004, mainly for the improvement of symptoms of ischemic cerebrovascular diseases caused by cerebral vasospasm after subarachnoid hemorrhage. [0003] Impurity control is one of the important contents of drug quality control. Whether the impurities in drugs can be fully and accurately...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/89G01N30/72G01N30/86G01N30/34G01N30/06
CPCG01N30/06G01N30/34G01N30/72G01N30/8634G01N30/89
Inventor 李宁陈云建刘世成李剑峰高宏涛
Owner KPC PHARM INC
Features
  • Generate Ideas
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com