A kind of detection method of ezetimibe intermediate

A detection method, the technology of ezetimibe, applied in the field of analytical chemistry, can solve the problems affecting the curative effect of drugs, affecting the chiral purity of ezetimibe isomer impurity content, etc., to achieve accurate and reliable calculation results, reliable detection methods, fast response effect

Active Publication Date: 2021-03-16
ENANTIOTECH CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The chiral purity and isomer impurities of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone will directly Affect the chiral purity of ezetimibe and the content of isomer impurities, thus directly affecting the efficacy of the drug
[0007] Currently, there is no chiral purity detection method for (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone In order to strengthen the quality control of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone, It is necessary to develop detection methods for

Method used

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  • A kind of detection method of ezetimibe intermediate
  • A kind of detection method of ezetimibe intermediate
  • A kind of detection method of ezetimibe intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A detection method for (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone,

[0039] 1. Instruments and testing conditions

[0040] Shimadzu LC-15C high performance liquid chromatography, the chromatographic column is chiralcel OD-H, its size is 4.6*250mm, 5μm;

[0041] Injection volume: 20μl;

[0042] Flow rate: 1ml / min;

[0043] Column temperature: 25°C;

[0044] Detection wavelength: 214nm;

[0045] Mobile phase: normal hexane: Virahol, its volume ratio is 700: 300;

[0046] Diluent: isopropanol;

[0047] Detector: UV detector.

[0048] 2. Experimental steps

[0049] Adopt high-performance liquid chromatography to detect, and the detection steps are as follows:

[0050] (1) Accurately weigh 25 mg of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone and 25 mg (4R)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone is placed in the same 100ml volumetric flask, Dissolve and dilute with diluent to prepare a syste...

Embodiment 2

[0055] Take three batches of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone produced according to the same production specifications, Test products 1-3 were tested according to the detection method of Example 1, and the area normalization method was used to calculate the purity and corresponding isomers. The test results are shown in the following table 1:

[0056] Table 1 is the detection result of test product 1-3

[0057]

[0058] figure 1It is the high performance liquid chromatogram of the system adaptability solution in embodiment 1, and the peak order is (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4- Phenyl-2-oxazolidinone, (4R)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone.

[0059] figure 2 It is the high performance liquid chromatogram of need testing product 1, and its detection result is shown in the following table 2. Wherein the peak at 23.174min is (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinon...

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Abstract

The invention discloses a detection method of an ezetimibe intermediate. According to the detection method, a high-performance liquid chromatograph is adopted for detection, an area normalization method is adopted for quantitative analysis, the chromatographic conditions are shown as follows: the chromatographic column is chiralcelOD-H, the sample amount is 15-25 mu l, the flow speed is 0.8-1.2 ml / min, the column temperature ranges from 20 DEG C to 30 DEG C, the detection wavelength is 210-220 nm, the mobile phase is n-hexane and isopropanol in the volume ratio being (960-1,000):20, a diluentis n-hexane and isopropanol in the volume ratio being (650-750):300, and a detector is an ultraviolet detector. By means of the detection method, rapid and accurate detection of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopenyl]-4-phenyl-2-oxazolidinone can be realized, the detection method has high sensitivity and is simple and convenient to operate, complete separation can be realized, and a basis for research, development and quality detection is provided for research of the compound.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a detection method of an ezetimibe intermediate. Background technique [0002] Ezetimibe (Ezetimble, chemical name: 1-(4-fluorophenyl)-(3R)-[3-(4-fluorophenyl)-(3S)-hydroxypropyl]-(4S)-(4 -Phenyl)-2-azetidinone) is a new type of cholesterol absorption inhibitor developed by Schering-Plough Pharmaceuticals, which was first launched in the United States in 2002 and is the first cholesterol absorption inhibitor approved by the FDA. [0003] [0004] (4S)-3-[5-(4-fluorophenyl)-5-hydroxy-1-oxopentyl]-4-phenyl-2-oxazolidinone is the key intermediate in the synthesis of ezetimibe . Its structural formula is: [0005] [0006] The chiral purity and isomeric impurities of (4S)-3-[5-(4-fluorophenyl)-1,5-dioxopentyl]-4-phenyl-2-oxazolidinone will directly Affect the chiral purity of ezetimibe and the content of isomer impurities, thereby directly affecting...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 蒙发明曹欢燕徐亮邓超芹俞伟文樊志麒
Owner ENANTIOTECH CORP
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