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

Method for measuring fat-soluble platinum complex and preparation related substances thereof

A technology for related substances and preparations, which is applied in the field of high-performance liquid chromatography to detect related substances in Miplatin raw materials and freeze-dried powder injection, and can solve the problems of difficulty in separating impurity A peak and solvent peak, impurity A cannot be effectively detected, etc.

Active Publication Date: 2015-05-06
SHINEWAY PHARMA GRP LTD
View PDF3 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant repeated the detection method for related substances provided by Chinese patent application 201410151902.5, and found that the chromatographic peak of impurity A overlapped with the solvent peak, and impurity A could not be effectively detected by using this chromatographic condition. It is difficult to separate the A peak and the solvent peak

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 measuring fat-soluble platinum complex and preparation related substances thereof
  • Method for measuring fat-soluble platinum complex and preparation related substances thereof
  • Method for measuring fat-soluble platinum complex and preparation related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Chromatographic conditions and system suitability test: octadecylsilane bonded silica gel as filler; mobile phase: A phase: methanol: ethanol (7:3), B phase: methanol: ethanol: water (7:3:40 ); flow rate 1.0mL / min; injection volume 20μL; column temperature 40°C; detection wavelength 210nm. The number of theoretical plates is not less than 2000 based on impurity A. Gradient times are as follows:

[0100] time (min)

A(v%)

B(v%)

0

85

15

[0101] 15

85

15

20

100

0

50

100

0

55

85

15

65

85

15

[0102] Determination method Take about 10mg of miplatin raw material, weigh it accurately, put it in a 10mL measuring bottle, add an appropriate amount of chromatographic ethanol and ultrasonically dissolve it, dilute it with ethanol to the mark, shake well, and filter it as the test solution. Take 20 μL each of the test solution, inject it into the liquid chrom...

Embodiment 2

[0123] Mobile phase: Phase A: methanol: ethanol (95:5), phase B: methanol: ethanol: water (95:5:400);

[0124] Gradient times are as follows:

[0125] time (min)

A(v%)

B(v%)

0

85

15

15

85

15

20

100

0

50

100

0

55

85

15

65

85

15

[0126] Other chromatographic conditions are the same as in Example 1.

[0127] Determination method Same as implementation 1.

[0128] The separation of the known impurity A and other unknown impurities in the rice platinum raw material by this method is greater than 1.5, which meets the requirements.

[0129] method validation

[0130] A. System suitability experiment:

[0131] Take the impurity A reference substance, according to the above chromatographic conditions, continuously inject 5 needles, the RSD of the impurity A peak area in the reference substance solution is 5.87%, the number of theoretical plates is 3491, and the system ...

Embodiment 3

[0149] Mobile phase: Phase A: methanol: ethanol (75:25), phase B: methanol: ethanol: water (75:25:400);

[0150] Gradient times are as follows:

[0151] time (min)

A(v%)

B(v%)

0

90

10

15

90

10

20

100

0

50

100

0

55

90

10

65

90

10

[0152] Other chromatographic conditions are the same as in Example 1.

[0153] The assay method is the same as that in Embodiment 1, except that the test sample is the freeze-dried powder of miplatin.

[0154] The separation of the known impurity A and other unknown impurities in the lyophilized powder of miplatin by this method is greater than 1.5, which meets the requirements.

[0155] method validation

[0156] A. System suitability experiment:

[0157] Take the impurity A reference substance, according to the above chromatographic conditions, continuously inject 5 needles, the RSD of the impurity A peak area in the reference subst...

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
recovery rateaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for measuring fat-soluble platinum complex and preparation related substances thereof. The detection method refers to a high performance liquid chromatography method. The chromatographic conditions are that the chromatographic column refers to an octadecylsilane chemically bonded silica (C18) chromatographic column; the phase A refers to a methanol-ethanol mixed solvent; the phase B refers to a mixed solvent of water and methanol or ethanol, and gradient elution is performed; the column temperature is 38-42 DEG C; the detection wavelength is 208-215nm; and the flow velocity is 0.5-2.0ml / min. With the adoption of the high performance liquid chromatography method disclosed by the invention, the content of impurities A and the content of other unknown impurities in the sample can be accurately determined, the separation degree of each impurity is high in the analysis process, the reproducibility of the analysis result is high, and a simple and reliable method is provided for quality control and analysis of miriplatin and preparations thereof.

Description

technical field [0001] The invention relates to a method for detecting related substances of miplatin raw materials and preparations thereof, more specifically a method for detecting related substances in miplatin raw materials and freeze-dried powder injections by high performance liquid chromatography. Background technique [0002] The so-called "related substances" in drug analysis refer to substances that are not the main components in a specific drug, but are related to the ingredients. Because a drug has to go through a relatively complicated and lengthy process from the synthesis of raw materials to the preparation of related preparations, storage, transportation, and use, during this period, each process may produce related substances, such as production. Starting materials, reagents, intermediates, by-products and isomers may be brought in; during storage and transportation, special impurities such as degradation products, polymers or crystal transformations may be ...

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
Inventor 郭勇南艳平郝福邵玉平李志刚
Owner SHINEWAY PHARMA GRP LTD
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