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Method for determining genotoxic substance ethyl chloroformate in loratadine by using gas chromatography

A technology of ethyl chloroformate and gas chromatography, which is applied in the field of separation and determination of genotoxic ethyl chloroformate in loratadine by gas chromatography, and can solve problems such as incomplete removal of genotoxic substances and affecting drug safety

Inactive Publication Date: 2020-12-22
AVENTIS PHARMA HAINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Incomplete removal of genotoxic substances in loratadine will seriously affect the safety of the drug

Method used

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  • Method for determining genotoxic substance ethyl chloroformate in loratadine by using gas chromatography
  • Method for determining genotoxic substance ethyl chloroformate in loratadine by using gas chromatography
  • Method for determining genotoxic substance ethyl chloroformate in loratadine by using gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Apparatus and conditions

[0037]Chromatograph: Agilent 6890N gas chromatograph;

[0038]Detector: hydrogen flame ionization detector;

[0039]Column: Polyethylene glycol polar capillary column;

[0040]Inlet temperature: 220℃;

[0041]Detector temperature: 300℃;

[0042]Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0043]Split ratio: 5:1;

[0044]Injection volume: 1μL

[0045]Oven heating program:

[0046] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 500 102005

[0047]Experimental steps

[0048]Take 100mg~200mg of loratadine, add 1.0mL solvent, shake well, sonicate, centrifuge, take the supernatant as the test solution; take an appropriate amount of ethyl chloroformate, dissolve it with a solvent, and make up to 1mL Ethyl chloroformate 9.5~19.0mg reference substance solution; take another 100mg~200mg of loratadine, add 1.0mL reference substance solution, shake well, ultrasound, centrifuge, take the supernatant, make up every 1mL containing ethyl chloroformate System suitability solution of est...

Embodiment 2

[0050]Apparatus and conditions

[0051]Chromatograph: Agilent 6890N gas chromatograph;

[0052]Detector: hydrogen flame ionization detector;

[0053]Column: Polyethylene glycol polar capillary column;

[0054]Inlet temperature: 220℃;

[0055]Detector temperature: 300℃;

[0056]Carrier gas (nitrogen) flow rate: 1.2mL / min;

[0057]Split ratio: 5:1;

[0058]Injection volume: 1μL

[0059]Oven heating program:

[0060] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 500 102005

[0061]Experimental steps

[0062]Take an appropriate amount of ethyl chloroformate and dissolve it with a solvent to prepare a reference solution containing 9.5-19.0mg of ethyl chloroformate per 1mL; take another 100mg~200mg of loratadine, add 1.0mL reference solution, and shake well , Sonication, centrifugation, take the supernatant and prepare a system suitability solution containing 9.5-19.0mg of ethyl chloroformate per 1mL. Take the system suitability solution, analyze according to the above chromatographic conditions, and record t...

Embodiment 3

[0064]Apparatus and conditions

[0065]Chromatograph: Agilent 6890N gas chromatograph;

[0066]Detector: hydrogen flame ionization detector;

[0067]Column: Polyethylene glycol polar capillary column;

[0068]Inlet temperature: 220℃;

[0069]Detector temperature: 300℃;

[0070]Carrier gas (nitrogen) flow rate: 1.0mL / min;

[0071]Split ratio: 10:1;

[0072]Injection volume: 1μL

[0073]Oven heating program:

[0074] Heating rate (℃ / min) Temperature (℃) Holding time (min) / 500 102005

[0075]Experimental steps

[0076]Take 100mg~200mg of loratadine, add 1.0mL of reference solution, shake well, ultrasound, centrifuge, take the supernatant, and prepare a system-suitable solution containing 9.5~19.0mg of ethyl chloroformate per 1mL. Take the system suitability solution, analyze according to the above chromatographic conditions, and record the chromatogram. The results are attachedFigure 6 , The chromatographic peak with retention time 5.703 min in the figure is ethyl chloroformate.

[0077]The present invention verifies t...

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PUM

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a method for separating and detecting a genotoxic substance ethyl chloroformate in loratadine by using gas chromatography, wherein the method adopts a polyethylene glycol polar capillary chromatographic column and a hydrogen flame ionization detector to quantitatively determine the content of the genotoxic substance ethyl chloroformate in loratadine. Therefore, the ethyl chloroformate in the loratadine is effectively controlled, and the quality of the loratadine is controllable. The method disclosed by the invention is strong in specificity, high in accuracy, good in durability and simple and rapid to operate.

Description

Technical field[0001]The invention belongs to the field of analytical chemistry, and specifically relates to a method for separating and determining the genotoxic substance ethyl chloroformate in loratadine by gas chromatography.Background technique[0002]Loratadine is an H1 receptor blocker. It is highly selective for peripheral H1 receptors and has a weak affinity for central H1 receptors. It can inhibit the release of leukotrienes and histamine from mast cells. It is a second-generation long-acting Tricyclic antihistamines. The zwitterionic characteristics in the molecular structure of loratadine make it have no obvious central inhibitory effect. It is mainly used to prevent and treat allergic rhinitis, chronic idiopathic urticaria, allergic asthma and specificity. Diseases such as dermatitis. The chemical name of Loratadine is 4-(8-chloro-5,6-dihydro-11H-benzo[5,6]cyclohepta[1,2-b]pyridine-11-ylidene)-1- Ethyl piperidine carboxylate, molecular formula C22H23CIN2O2, The structural...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025
Inventor 张丽娜刘秋叶孙冬雪
Owner AVENTIS PHARMA HAINAN
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