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Determination method for dehydrophenylahistins analogue and isomers thereof

A technology of analogs and isomers, applied in the field of drug analysis, can solve problems such as difficult separation and detection

Active Publication Date: 2018-12-18
SHENZHEN NEPTUNUS PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, dehydrophenylahistine analogs and their isomer impurities are difficult to separate and detect, and there are no related literature reports so far

Method used

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  • Determination method for dehydrophenylahistins analogue and isomers thereof
  • Determination method for dehydrophenylahistins analogue and isomers thereof
  • Determination method for dehydrophenylahistins analogue and isomers thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of dehydrophenylahistine analogues for testing:

[0050] The test sample of dehydrophenylahistine analogue (I) was prepared with reference to Example 3 of the specification of patent application CN 106565686A.

Embodiment 2

[0052] Prepare the reference substance of dehydrophenylahistine analog (I):

[0053] Use acetone recrystallization to obtain the test sample of the dehydrophenylahistine analogue (I) obtained in Example 1, and dry to obtain the reference substance of the dehydrophenylahistine analogue (I), the purity 99.1%, batch number: 20170710.

Embodiment 3

[0055] Prepare the reference substance of impurity B:

[0056] Take 3-(3-fluoro)phenylacrolein and (Z)-1-acetyl-3-((5-(tert-butyl)-1H-imidazol-4-yl)methylene)piperazine-2 , 5-diketone synthesis, the synthesis conditions refer to the publication number CN 106565686A in Example 3 Step 3. Purity 98.0%, batch number: 20171012.

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Abstract

The invention discloses a high performance liquid chromatography method for simultaneously determining the content of a dehydrophenylahistins analogue and a plurality of isomers thereof, wherein the dehydrophenylahistins analogue is (3Z, 6Z)-3-((E)-3-(5-tert-butyl)-1H-imidazol-4-yl)methylene)-6-((E)-3-(3-fluorophenyl)-2-propenylidene)piperazine-2,5-dione. The specific detection method comprises the steps of adopting a chromatographic column of pentafluorophenyl to chemically bond a silica gel column (250 x 4.6 mm, 4 [mu]m), adopting water-methanol as mobile phase, and carrying out isocratic elution, wherein the column temperature is 50 DEG C, the flow rate is 1.0 ml / min, and the detection wavelength is 375 nm. The determination method for the dehydrophenylahistins analogue and the isomers thereof can rapidly and accurately detect the content of the dehydrophenylahistins analogue and the plurality of isomers thereof, is simple to operate, good in reproducibility, and high in sensitivity, and provides the quality assurance for drug substance and preparation development of the dehydrophenylahistins analogue.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for detecting compounds and their isomers by high performance liquid chromatography. Background technique [0002] Chinese patent application CN 106565685A discloses a series of dehydrophenylahistine analogs and their preparation methods. These compounds have a substituted heterocyclic skeleton and have tubulin inhibitory activity. The base-binding site is the target, and it is planned to be used in combination with the chemotherapy agent docetaxel in the preparation of drugs for the treatment of tumors. The dehydrophenylahistine analogue of the present invention is (3Z,6Z)-3-((E)-3-(5-tert-butyl)-1H-imidazolyl-4-yl)methylene Base)-6-((E)-3-(3-fluorophenyl)-2-propenylidene)piperazine-2,5-dione, the molecular formula is C 21 h 21 FN 4 o 2 , its chemical structural formula is as shown in (I): [0003] [0004] 3-(3-fluoro)phenylacrolein is the starting material for th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 陈艳萍郭青石涛唐田卢禁王彦青吴婧王志国杨经安
Owner SHENZHEN NEPTUNUS PHARMA RES INST CO LTD