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

Method for separation determination of posaconazole intermediate Z1 and related substances of posaconazole intermediate Z1

A related substance, posaconazole technology, applied in the field of analytical chemistry, to achieve the effect of strong specificity and high sensitivity

Inactive Publication Date: 2016-05-25
CHONGQING HUAPONT PHARMA
View PDF8 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to control the quality of posaconazole intermediate Z1, it is necessary to separate and measure posaconazole intermediate Z1 and its related substances. At present, there is no published method to report the separation and determination of posaconazole intermediate Z1 and its related substances. method

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 separation determination of posaconazole intermediate Z1 and related substances of posaconazole intermediate Z1
  • Method for separation determination of posaconazole intermediate Z1 and related substances of posaconazole intermediate Z1
  • Method for separation determination of posaconazole intermediate Z1 and related substances of posaconazole intermediate Z1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1 The method for the determination of related substances in posaconazole intermediate Z1 by high performance liquid chromatography

[0071] Specific method steps:

[0072] 1) Prepare a blank solution: take 40ml of water, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0073] 2) Prepare related substance localization solution: take posaconazole intermediate Z1 related substance reference substance, dissolve and dilute with diluent to obtain impurity localization solution;

[0074] 3) Prepare the test solution: take about 50 mg of posaconazole intermediate Z1, accurately weigh it, put it in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0075] 4) Prepare self-contrast solution: accurately pipette 1.0ml of the test solution, put it in a 100ml measuring bottle, add diluent to dilute to the mark, shake well, then precisely pipette 1.0...

Embodiment 2

[0077] Example 2 The separation degree of the chromatographic system of the present invention to posaconazole intermediate Z1 and its related substances

[0078] Specific method steps:

[0079] 1) Prepare a blank solution: take 40ml of water, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0080] 2) Prepare the test solution: accurately weigh 149.85 mg of intermediate Z, put it in a 25 ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and obtain; (1.994 mg / ml);

[0081] 3) Preparation of related substance positioning solution:

[0082] a) Impurity 1 stock solution: Accurately weigh 112.71mg of impurity, put it in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and obtain; (508.4μg / ml);

[0083] b) Impurity 2 stock solution: Accurately weigh 212.70mg of impurity, put it in a 25ml measuring bottle, add diluent to dissolve and dilute to the mark, shake w...

Embodiment 3

[0090] Example 3 The system suitability test of the chromatographic system of the present invention to the posaconazole intermediate Z1

[0091] experiment procedure:

[0092] 1) Prepare a blank solution: take 40ml of water, put it in a 100ml measuring bottle, add acetonitrile to dilute to the mark, shake well, and you get it;

[0093] 2) Preparation of the test solution: take posaconazole intermediate Z149.85mg, accurately weighed, put in a 25ml measuring bottle, add diluent to dissolve and dilute to the scale, shake well, and obtain;

[0094] 3) Prepare self-contrast solution: accurately pipette 1.0ml of the test solution, put it in a 100ml measuring bottle, add diluent to dilute to the mark, shake well, then precisely pipette 1.0ml, put it in a 10ml measuring bottle, add diluent to dilute to the scale, shake well, and you get it; (0.1%);

[0095] 4) Take the self-control solution and inject 6 needles continuously, record the chromatogram, see Figure 4 Calculate the peak...

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
Login to View More

Abstract

The invention belongs to the analytical chemistry filed, in particular to a method for separation determination of a posaconazole intermediate Z1 and related substances of the posaconazole intermediate Z1. Octadecylsilane chemically bonded silica is used as a chromatographic column of a filler, and an inorganic salt buffer solution and an organic solvent are taken as mobile phases for solid-liquid separation; the method can fully separate the posaconazole intermediate Z1 and the related substances of the posaconazole intermediate Z1, the solvent peak doesn't interfere with the posaconazole intermediate Z1 and the related substances of the posaconazole intermediate Z1 in detection, and the separation degree is larger than 1.5; the method is high in specificity, good in stability and high in sensibility and accuracy, the posaconazole intermediate Z1 and the related substances of the posaconazole intermediate Z1 can be separated effectively, and the quality safety of posaconazole raw materials and preparations of the posaconazole raw materials is guaranteed; the operation method is simple, has the advantages that the method is easy, convenient and rapid and has vitally important significance to quality control and safety guarantee of the posaconazole intermediate Z1.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring posaconazole intermediate Z1 and its related substances. Background technique [0002] Posaconazole, a broad-spectrum triazole antifungal, is indicated for the prophylaxis of invasive Aspergillus and Candida infections and for the treatment of oropharyngeal candidiasis, including itraconazole and or fluconazole refractory Oropharyngeal candidiasis. Posaconazole intermediate Z1 chemical name: 4-(4-(4-(4-(((3R,5R)-5-((1H-1,2,4-triazol-1-yl)methyl) Base)-5-(2,4-difluorophenyl)tetrahydrofuran-3-yl)methoxy)phenyl)piperazin-1-yl)phenyl)-1-((2S,3S)-2- (Phenoxy)pentan-3-yl)-1H-1,2,4-triazol-5(4H)-one, molecular formula: C 44 h 48 f 2 N 8 o 4 , molecular weight: 790.9, structural formula: [0003] [0004] During the synthesis of posaconazole, its intermediate Z1 may have several key process impurities and reaction by-product...

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): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 李江玲沈红梅
Owner CHONGQING HUAPONT 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