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Method for determining solvents residual in ezetimibe bulk drug through headspace gas chromatography

A headspace gas chromatography and ezetimibe technology, which is applied in the field of drug analysis, can solve problems that need to be improved, and achieve rapid and efficient separation and content determination, convenient operation, and high precision.

Active Publication Date: 2018-03-30
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the method for the determination of residual solvents in ezetimibe raw materials still needs to be improved

Method used

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  • Method for determining solvents residual in ezetimibe bulk drug through headspace gas chromatography
  • Method for determining solvents residual in ezetimibe bulk drug through headspace gas chromatography
  • Method for determining solvents residual in ezetimibe bulk drug through headspace gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0051] Chromatographic column: KB-624 (30m*0.32mm, 3.0μm);

[0052] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 1.0ml / min; split ratio: 1:1;

[0053] Detector temperature: 250°C; inlet temperature: 200°C;

[0054] Column temperature: the initial temperature is 40°C for 15 minutes, then rise to 200°C at a rate of 10°C / min, and hold for 8 minutes.

[0055] Headspace detection parameters: heating box temperature: 90℃; quantitative loop temperature: 100℃; transmission line temperature: 110℃;

[0056] Headspace balance time: 30min; cycle time: 50min; sampling time: 0.5min;

[0057] Pressure balance time: 0.1min.

[0058] 1. Exclusiveness

[0059] Blank solution: dimethyl sulfoxide (DMSO).

[0060] Methanol stock solution: Take about 750mg of methanol, accurately weigh it, put it in a 25ml measuring flask, dilute and dissolve with DMSO to the mark, shake well, and get it;

[0061] Isopr...

Embodiment 2

[0093] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0094] Chromatographic column: KB-624 (30m*0.32mm, 3.0μm);

[0095] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 1.2ml / min; split ratio: 1:1;

[0096] Detector temperature: 250°C; inlet temperature: 200°C;

[0097] Column temperature: the initial temperature is 40°C for 15 minutes, then rise to 200°C at a rate of 10°C / min, and hold for 8 minutes.

[0098] Headspace detection parameters: heating box temperature: 90℃; quantitative loop temperature: 100℃; transmission line temperature: 110℃;

[0099] Headspace balance time: 30min; cycle time: 50min; sampling time: 0.5min;

[0100] Pressure balance time: 0.1min.

[0101] experiment procedure:

[0102] Blank solution: dimethyl sulfoxide (DMSO).

[0103] System suitability solution: Precisely pipette 1.0 ml of each positioning solution in Example 1 into a 100 ml volumetric flask containing about 30 ml of DMSO, dilute to the mark with th...

Embodiment 3

[0108] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0109] Chromatographic column: KB-624 (30m*0.32mm, 3.0μm);

[0110] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 0.8ml / min; split ratio: 1:1;

[0111] Detector temperature: 250°C; inlet temperature: 200°C;

[0112] Column temperature: the initial temperature is 40°C for 15 minutes, then rise to 200°C at a rate of 10°C / min, and hold for 8 minutes.

[0113] Headspace detection parameters: heating box temperature: 90℃; quantitative loop temperature: 100℃; transmission line temperature: 110℃;

[0114] Headspace balance time: 30min; cycle time: 50min; sampling time: 0.5min;

[0115] Pressure balance time: 0.1min.

[0116] experiment procedure:

[0117] Blank solution: dimethyl sulfoxide (DMSO).

[0118] System suitability solution: Precisely pipette 1.0 ml of each positioning solution in Example 1 into a 100 ml volumetric flask containing about 30 ml of DMSO, dilute to the mark with th...

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Abstract

The invention discloses a method for determining solvents residual in an ezetimibe bulk drug The method adopts the following analysis conditions: the chromatographic column adopts a capillary chromatographic column with 6% cyanopropylphenyl 94% polydimethylsiloxane as the stationary phase; a reference substance solution is injected multiple times in a split flow manner, a sample solution is injected in the split flow manner, the carrier gas is nitrogen, the introduction is carried out by using a headspace injector, and detection is performed after temperature programming; and the detector adopts an FID detector. Methanol, isopropanol, fluorobenzene, toluene and N,N-dimethyl formamide in the ezetimibe bulk drug are rapidly and efficiently separated under same chromatographic conditions through the method in order to effectively control the quality of ezetimibe. The detection method has the advantages of strong specificity, high detection sensitivity, high precision, high accuracy, convenience in operation, and effective control of the product quality.

Description

Technical field [0001] The present invention belongs to the technical field of pharmaceutical analysis. Specifically, the present invention relates to a method for measuring residual solvents in ezetimibe bulk medicine by using headspace gas chromatography. Background technique [0002] The chemical name of the raw material of ezetimibe is (4S)-3-[(5S)-5-(4-fluorophenyl)-5-hydroxyvaleryl]-4-phenyl-1,3-oxazepine Pentan-2-one, its structural formula is: [0003] [0004] The organic solvents that are used in the production of raw materials and preparations of pharmaceuticals but are not completely removed are collectively referred to as residual solvents. If the residual amount exceeds a safe value, it will have a certain impact on the patient's body. The ICH guidelines specify 4 types of solvents and their limit values ​​according to the degree of hazard. According to the requirements for residual solvent content and the synthesis process of ezetimibe API in the fourth part of the...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/16
CPCG01N30/02G01N30/16
Inventor 高宏平杭健孙梦颖钱丽娜
Owner WATERSTONE PHARMA WUHAN
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