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

Detection method of acetylcysteine enantiomer

A technology for acetylcysteine ​​and enantiomers, applied in the field of analysis and detection, can solve the problems of low accuracy, insufficient separation of chromatographic peaks of isomers, etc.

Pending Publication Date: 2022-07-01
SICHUAN HUIYU PHARMA +1
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing detection method, the resolution of isomer chromatographic peaks is insufficient, and the detection accuracy is low

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
  • Detection method of acetylcysteine enantiomer
  • Detection method of acetylcysteine enantiomer
  • Detection method of acetylcysteine enantiomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Prepare the solution

[0038] Test solution: Measure 1.5ml of Acetylcysteine ​​Injection, put it in a 20ml measuring bottle, add diluent (ethanol-isopropanol=60:40v / v) to dilute to the mark, shake well, and use it as the test product solution.

[0039] Spiked test solution: Measure 1.5ml of Acetylcysteine ​​Injection, put it in a 20ml volumetric bottle, add 2ml of the reference substance stock solution precisely, add diluent to dilute to the mark, shake well, and use it as the spiked test solution . 6 copies were prepared in parallel.

[0040] Reference substance solution: take 5.6 mg of the isomer reference substance, accurately weigh it, put it in a 25ml measuring bottle, add a diluent to dissolve and dilute to the mark, shake well, and use it as the reference substance stock solution, accurately measure 2ml of the reference substance stock solution, Put it in a 20ml measuring bottle, add diluent to dilute to the mark, shake well, and use it as a reference solut...

Embodiment 2

[0067] 1. Preparation of solution (same as Example 1)

[0068] 2. HPLC detection

[0069] Diluent: ethanol: isopropanol = 60:40 (volume ratio)

[0070] Mobile phase: n-hexane: isopropanol: ethanol: trifluoroacetic acid = 88:10:2:0.1 (volume ratio)

[0071] Column: CHIRALPAK IG, 4.6×250mm, 5μm

[0072] Detection wavelength: 205nm

[0073] Column temperature: 30℃

[0074] Flow rate: 1.5ml / min

[0075] 2.1 Chromatogram

[0076] Precisely measure 10 μl of the test solution, inject the sample, and record the chromatogram as follows figure 2 . according to figure 2 , the number of plates is 5857, and the degree of separation is 3.8.

[0077] 2.2 Repeatability

[0078] Precisely measure 6 doses of 10 μL of the standard solution of the test sample, inject the sample, record the chromatogram, and calculate the result according to the chromatogram:

[0079] sample 1 2 3 4 5 6 RSD Recovery rate 100.8 101.9 103.2 101.0 102.8 102.5 0.96％ degr...

Embodiment 3

[0087] 1. Preparation of solution (same as Example 1)

[0088] 2. HPLC detection

[0089] Diluent: ethanol: isopropanol = 60:40 (volume ratio)

[0090] Mobile phase: n-hexane: isopropanol: ethanol: trifluoroacetic acid = 92:6:2:0.1 (volume ratio)

[0091] Column: CHIRALPAK IG, 4.6×250mm, 5μm

[0092] Detection wavelength: 205nm

[0093] Column temperature: 30℃

[0094] Flow rate: 1.5ml / min

[0095] 2.1 Chromatogram

[0096] Precisely measure 10 μl of the test solution, inject the sample, and record the chromatogram as follows image 3 . according to image 3 , the number of trailing trays is 6633, and the degree of separation is 4.7.

[0097] 2.2 Repeatability

[0098] Precisely measure 6 doses of 10 μL of the standard solution of the test sample, inject the sample, record the chromatogram, and calculate the result according to the chromatogram:

[0099] sample 1 2 3 4 5 6 RSD Recovery rate 103.6 102.1 101.2 100.5 102.8 104.3 1.4％ ...

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
Wavelengthaaaaaaaaaa
Wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention relates to the technical field of analysis and detection, in particular to a detection method of acetylcysteine enantiomers. The detection method of the acetylcysteine enantiomer provided by the invention comprises the following steps: diluting a sample with a diluent, and carrying out HPLC (High Performance Liquid Chromatography) detection, the diluent is composed of ethanol and isopropanol; chromatographic conditions of the HPLC detection are as follows: a chromatographic column is a chiral column; a mobile phase is composed of normal hexane, isopropanol, ethanol and trifluoroacetic acid, and isocratic elution is carried out. When the method provided by the invention is used for detection, the pretreatment steps of the sample can be reduced. The detection result shows that the method provided by the invention can enable the L-acetylcysteine and the D-acetylcysteine to have better separation degree, and the accuracy, the sensitivity, the repeatability and the precision of the detection are all good.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for detecting acetylcysteine ​​enantiomers. Background technique [0002] Acetylcysteine ​​is a mucolytic agent with strong phlegm-dissolving effect. The sulfhydryl group contained in the molecule can break the disulfide bond in the glycoprotein polypeptide chain in the sputum, thereby reducing the viscosity of the sputum and making the sputum liquefied and easy to cough up. It can also break DNA fibers in purulent sputum, so it can not only dissolve white sticky sputum, but also purulent sputum. Acetylcysteine ​​contains a chiral center and contains two configurations, L configuration and D configuration, wherein the L configuration is an effective configuration, and the D configuration should be controlled as an impurity. [0003] At present, the pharmaceutical dosage forms of acetylcysteine ​​circulating on the market include oral preparations, inject...

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): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679
Inventor 刘红莲丁兆胡和平付训忠王爱丽毛灵慧张吉旺
Owner SICHUAN HUIYU PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com