Alpha-tropine related substance and isomer inspecting method

A technology related to substances and inspection methods, applied in the direction of analysis by chemical reaction of materials, and material analysis by observing the effect on chemical indicators, which can solve the problems of small molecular weight, large alkalinity, peak area and peak shape weight. Problems such as poor performance, to achieve the effect of simple operation

Inactive Publication Date: 2017-11-07
SHANDONG QIDU PHARMA
View PDF3 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, tropinol and its analogues have small molecular weight, high alkalinity, strong polarity, and no UV absorption. In the development of gas-phase methods, the separation between isomers and main components is good with DB-1, but the peak Area and peak shape reproducibility is poor

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
  • Alpha-tropine related substance and isomer inspecting method
  • Alpha-tropine related substance and isomer inspecting method
  • Alpha-tropine related substance and isomer inspecting method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take an appropriate amount of α-tropine alcohol, weigh it accurately, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 2mg / ml, as the test solution.

[0020] Take an appropriate amount of β-tropine alcohol and tropinone, accurately weighed, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 10 μg / ml, as a reference solution.

[0021] Take 10 μl each of the above-mentioned test solution and reference solution, respectively spot on the same silica gel HSGF254 plate, develop with a developer of dichloromethane:methanol:water:isopropylamine=55:40:5:3, and dry with cold air.

[0022] When developing color, first evenly spray sulfuric acid modified bismuth iodide potassium test solution on the thin-layer plate, dry it with cold air, and continue to spray sodium nitrite test solution; preparation method of bismuth potassium iodide test solution: A liquid: take bismuth subnitrate / basic fo...

Embodiment 2

[0026] Take an appropriate amount of α-tropine alcohol, weigh it accurately, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 1 mg / ml, as the test solution.

[0027] Take an appropriate amount of β-tropine alcohol and tropinone, accurately weighed, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 5 μg / ml, as a reference solution.

[0028] Take 5 μl of each of the above-mentioned test solution and reference solution, spot on the same silica gel HSGF254 plate, develop with a developer of dichloromethane:methanol:water:diethylamine=50:35:4:2, and dry with cold air.

[0029] When developing color, first evenly spray sulfuric acid modified bismuth iodide potassium test solution on the thin-layer plate, dry it with cold air, and continue to spray sodium nitrite test solution; preparation method of bismuth potassium iodide test solution: A liquid: take bismuth subnitrate / basic formula Bismut...

Embodiment 3

[0033] Take an appropriate amount of α-tropine alcohol, weigh it accurately, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 2mg / ml, as the test solution.

[0034] Take an appropriate amount of β-tropine alcohol and tropinone, accurately weighed, add dichloromethane-methanol (1:1) to dissolve and dilute to a solution with a concentration of 8 μg / ml, as a reference solution.

[0035] Take 10 μl each of the above-mentioned test solution and reference solution and spot on the same silica gel HSGF254 plate, develop with a developer of dichloromethane:methanol:water:isopropylamine=58:45:5:5, and dry with cold air.

[0036] When developing color, first evenly spray sulfuric acid modified bismuth iodide potassium test solution on the thin-layer plate, dry it with cold air, and continue to spray sodium nitrite test solution; preparation method of bismuth potassium iodide test solution: A liquid: take bismuth subnitrate / basic formula Bism...

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

No PUM Login to view more

Abstract

The invention discloses a method for inspecting alpha-tropine related substance and isomer inspecting method by a thin-layer chromatography. By means of preparing a related substance and isomer reference substance solution, a sample loading amount is controlled; after a developer is spread, a color developing agent is sprayed; thus, tropine related substance and isomer can be controlled under 0.5%. The method has the advantages of simpleness in operation, convenience and quickness; dedicated inspecting instruments are avoided; an economical, practical and effective method is provided for quick detection on tropine.

Description

technical field [0001] The invention relates to a method for checking alpha-tropine related substances and isomers, and belongs to the technical field of drug analysis. Background technique [0002] Tropisetron hydrochloride is a highly efficient and highly selective competitive antagonist of peripheral neurons and central nervous system 5-hydroxytryptamine 3 (5-HT3) receptors, which is used for the prevention and treatment of nausea and vomiting caused by cancer chemotherapy. Currently, the dosage forms listed in China include tablets, capsules and injections. [0003] Tropinol is a starting material for the synthesis of tropisetron, and its isomer β-tropine and related substance tropinone are taken as important control objects in the quality control to ensure the efficacy of tropisetron hydrochloride. However, tropinol and its analogues have small molecular weight, high alkalinity, strong polarity, and no UV absorption. In the development of gas-phase methods, although th...

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
Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78
Inventor 李德凤张涛孔令金刘海萍刘文坤
Owner SHANDONG QIDU PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap