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

Preparation method of cilastatin sodium impurity C

A technology for cilastatin sodium and impurities, which is applied in the field of preparation of cilastatin sodium impurity C, can solve problems such as affecting drug efficacy, and achieve the effects of low cost, optimized synthesis process and high yield

Inactive Publication Date: 2020-08-21
LIVZON NEW NORTH RIVER PHARMA
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The presence of impurities can seriously affect the efficacy of the drug

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
  • Preparation method of cilastatin sodium impurity C
  • Preparation method of cilastatin sodium impurity C
  • Preparation method of cilastatin sodium impurity C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Methanol and DMSO are mixed into solvent according to the volume ratio of 1:1, and the former drug of dissolving cilastatin sodium makes the final concentration of cilastatin sodium be 250mg / ml, as need testing solution; Carry out high-pressure liquid chromatography mass spectrometry to obtain the peak entry time and peak exit time of cilastatin sodium impurity C;

[0056] High performance liquid chromatography-mass spectrometer: Thermo LCQ FLEET; Chromatographic column: Agilent ZORBAX SB-Aq, 4.6×250mm, 5μm;

[0057] Mobile phase A is an aqueous solution containing 0.1% formic acid; mobile phase B is acetonitrile;

[0058] Gradients are set to:

[0059]

[0060] The flow rate is 1mL / min; the detection wavelength is 210nm; the injection volume: 20μl.

[0061] From the obtained chromatogram, the peak entry time and peak exit time of cilastatin sodium impurity C are 64.5, 65.4min respectively. The high-pressure liquid chromatography-mass spectrometry in this part...

Embodiment 2

[0079] (1) methanol and DMSO are mixed into a solvent according to the volume ratio of 1:1.2, and the former drug of cilastatin sodium is dissolved so that the final concentration of cilastatin sodium is 240mg / ml, as the test solution; Carry out high-pressure liquid chromatography mass spectrometry to obtain the peak entry time and peak exit time of cilastatin sodium impurity C;

[0080] High pressure liquid chromatography mass spectrometry parameters:

[0081] High performance liquid chromatography-mass spectrometer: Thermo LCQ FLEET; Chromatographic column: Agilent ZORBAX SB-Aq4.6×250mm, 5μm;

[0082] Mobile phase A is an aqueous solution containing 0.1% formic acid; mobile phase B is acetonitrile;

[0083] Gradients are set to:

[0084]

[0085] The flow rate is 1mL / min; the detection wavelength is 210nm; the injection volume: 20μl.

[0086] From the obtained chromatogram, the peak entry time and peak exit time of cilastatin sodium impurity C are 64.5, 65.4min respect...

Embodiment 3

[0101](1) methanol and DMSO are mixed into solvent according to the volume ratio of 1:1.5, and the former medicine of dissolving cilastatin sodium makes the final concentration of cilastatin sodium be 255mg / ml, as need testing solution; Carry out high-pressure liquid chromatography mass spectrometry to obtain the peak entry time and peak exit time of cilastatin sodium impurity C;

[0102] High pressure liquid chromatography mass spectrometry parameters:

[0103] High performance liquid chromatography-mass spectrometer: Thermo LCQ FLEET; Chromatographic column: Agilent ZORBAX SB-Aq, 4.6×250mm, 5μm;

[0104] Mobile phase A is an aqueous solution containing 0.1% formic acid; mobile phase B is acetonitrile;

[0105] Gradients are set to:

[0106]

[0107] The flow rate is 1mL / min; the detection wavelength is 210nm; the injection volume: 20μl.

[0108] From the obtained chromatogram, the peak entry time and peak exit time of cilastatin sodium impurity C are 64.5, 65.4min resp...

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 preparation method of a cilastatin sodium impurity C. The preparation method comprises the steps of preparing a cilastatin sodium test solution, carrying out high-pressure liquid chromatography separation, concentrating, carrying out high-pressure liquid chromatography secondary separation, concentrating and drying to obtain the cilastatin sodium impurity C. Elution is carried out in a gradient manner, a mobile phase A is formic acid, and a mobile phase B is acetonitrile. The preparation method of the cilastatin sodium impurity C provided by the invention is short inperiod and high in detection sensitivity, has the advantages of being simple, rapid, high in purity, high in yield, low in cost and the like, and has important significance in quality control and pharmacology and toxicology research of cilastatin sodium.

Description

technical field [0001] The invention belongs to the field of drug analysis and detection, and relates to a preparation method of impurity C of cilastatin sodium. Background technique [0002] Cilastatin sodium (Cilastatin sodium, CS) is a renal dehydropeptidase I inhibitor. Cilastatin sodium has no antibacterial activity and no inhibitory effect on β-lactamase. It is a carbocyanine A synergist of myprene drug imipenem (Imipenen, IMP). The structural formula of cilastatin sodium impurity C is: [0003] [0004] When imipenem IMP is administered alone, after glomerular filtration or secretion, imipenem is hydrolyzed by dehydropeptidase I in the brush border of proximal renal tubular epithelial cells, making imipenem inactive60 % to 95%, and even reduced the active drug concentration in urine. CS can inhibit the entry of IMP into the renal tubular epithelial tissue, reduce the excretion of IMP and the integrity of IMP in the kidney, prevent renal tubular necrosis caused b...

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): G01N30/06
CPCG01N30/06G01N2030/042
Inventor 王珂陈圳平陈倩倩张勇吴云香
Owner LIVZON NEW NORTH RIVER 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