A kind of method for separating and measuring Ribociclib and impurities

A ribociclib and impurity technology, applied in the field of analytical chemistry, can solve the problems of difficult to achieve effective separation of ribociclib, unfavorable to the quality control of ribociclib, increase the difficulty of detection, etc., and achieve accurate and reliable detection results. , eliminate solvent effect, improve the effect of separation

Active Publication Date: 2022-05-27
CHONGQING SANSHENG IND CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] It can be seen that Ribociclib has more impurities and similar structures, which makes separation difficult
In addition, the polarity of each impurity is different. On the premise of satisfying the separation between Ribociclib and each impurity, the separation between impurities must also be satisfied, which increases the difficulty of detection.
It is difficult to achieve effective separation between Ribociclib and impurities and between impurities and impurities by conventional detection methods, which is not conducive to the quality control of Ribociclib
[0007] This product is currently not on the market in China, and there is no authoritative report and detection method for relevant impurities

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
  • A kind of method for separating and measuring Ribociclib and impurities
  • A kind of method for separating and measuring Ribociclib and impurities
  • A kind of method for separating and measuring Ribociclib and impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take impurity Z1, impurity Z2, impurity Z3, impurity Z4, impurity Z5, impurity Z6, impurity Z7, impurity Z8, impurity Z9, impurity Z10, impurity Z11, impurity Z12, impurity Z13, impurity Z14 (the purity of each impurity is in More than 99%, each impurity is provided by Chongqing Sansheng Industrial Co., Ltd.) 25mg each, accurately weighed, placed in a 100ml measuring bottle, add acetonitrile-0.01mol / L potassium dihydrogen phosphate solution (pH is 3.0) (volume The ratio is 10:90) dissolved and diluted to the scale, shaken up, as the impurity stock solution; take about 25 mg of ribociclib (provided by Chongqing Sansheng Industrial Co., Ltd., the purity is 99.88%), accurately weighed, placed in In a 50ml volumetric flask, accurately add 1ml of the impurity stock solution, add acetonitrile-0.01mol / L potassium dihydrogen phosphate solution (pH is 3.0) (volume ratio is 10:90) to dissolve and dilute to the mark, shake well, as a mixed control solution .

[0035] Take the dil...

Embodiment 2

[0039] Example 2 Determination of ribociclib API (provided by Chongqing Sansheng Industrial Co., Ltd.)

[0040] Take ribociclib 25mg, accurately weigh it, put it in a 50ml measuring bottle, add (acetonitrile-0.01mol / L potassium dihydrogen phosphate solution (pH is 3.0)=10:90) ultrasonic treatment to dissolve and dilute to the mark, shake Evenly, as a sample solution; accurately measure 1ml of the sample solution, place it in a 100ml measuring bottle, dilute it to the mark with (acetonitrile-0.01mol / L potassium dihydrogen phosphate solution (pH 3.0)=10:90), shake well , as the control solution; carry out liquid chromatographic analysis according to the chromatographic conditions of Example 1, and record the chromatogram. If there are impurity peaks (except solvent peaks) in the chromatogram of the sample solution, calculate the impurity content according to the self-control method. The result is as image 3 , Figure 4 shown. The test results are shown in Table 1:

[0041]...

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
volume ratioaaaaaaaaaa
volume ratioaaaaaaaaaa
Login to view more

Abstract

A method for separating and measuring ribociclib and impurities, comprising the following steps, 1) taking ribociclib and dissolving it with a diluent to obtain a sample solution with a concentration of 0.1-10mg / ml; 2) taking the sample solution of step 1). Sample solution adds diluent and dilutes 50-1000 times, obtains contrast solution; 3) adopt octadecylsilane bonded silica gel to be the chromatographic column of filler, the flow velocity of setting mobile phase is 0.8-1.2ml / min, and mobile phase is by the concentration of 0.0001-1.0mol / L buffer solution and acetonitrile composition, adopts the gradient elution method to enter the chromatographic column; 4) Step 1) sample solution, step 2) control solution of equal volume are injected into the high performance liquid chromatograph respectively, The sample volume is 5μl-100μl, and the wavelength of 210nm to 290nm is used to detect, record the chromatogram, and complete the separation and determination of impurities in the sample solution. The invention is simple and convenient to operate, and can effectively realize the separation and measurement of ribociclib and impurities, impurities and impurities, thereby realizing the purpose of controlling the quality of ribociclib and its products.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and determining Ribociclib and impurities. Background technique [0002] Ribociclib is a novel drug developed by Novartis, which selectively inhibits CDK4 / 6, restores cell cycle control, and blocks tumor cell proliferation, thereby achieving breast cancer treatment. In March 2017, it was approved by the US FDA for listing, its trade name is Kisqali, and its chemical name is 7-cyclopentyl-N,N-dimethyl-2-[[5-(1-piperazinyl)-2- Pyridyl]amino]-7H-pyrrolo[2,3-D]pyrimidine-6-carboxamide succinate, the chemical structure of which is shown in formula (a). [0003] In the process of synthesizing this compound, there are several important intermediates and unknown impurities that may affect the purity and quality of the drug due to incomplete removal. These known intermediates and unknown impurities and the resulting degradation products are the drug quality con...

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 Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张洪兰潘呈恭潘先文杨欢代广会高亚朱思文彭艳
Owner CHONGQING SANSHENG IND CO LTD
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