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Method for detecting residual solvent in ibudilast bulk drug

A detection method and residual solvent technology are applied in the field of drug analysis and detection, which can solve problems such as organic solvent environment and human harm, and achieve the effects of controlling product quality, ensuring drug safety, and improving product quality.

Inactive Publication Date: 2020-06-30
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the research results released by authoritative organizations such as the World Health Organization, many organic solvents have certain harm to the environment and human body.

Method used

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  • Method for detecting residual solvent in ibudilast bulk drug
  • Method for detecting residual solvent in ibudilast bulk drug
  • Method for detecting residual solvent in ibudilast bulk drug

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Experimental program
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Embodiment

[0026] 1. Instruments and reagents

[0027] Instrument: Agilent 7890A gas chromatograph, detector: FID; Agilent chromatography workstation;

[0028] Reagents: All reagents used are chromatographically pure; ibudilast (self-made).

[0029] 2. Chromatographic conditions

[0030] Chromatographic column: Agilent DB-624 (30m×0.53mm, 3.0μm);

[0031] Column temperature: keep at 35°C for 4 minutes, increase to 200°C at a rate of 45°C / min, and keep for 10 minutes;

[0032] Injection port temperature: 200°C;

[0033] Detection temperature: 220°C;

[0034] Carrier gas: N 2 , split ratio: 10:1;

[0035] Sampling method: headspace sampling method;

[0036] Balance time: 20min;

[0037] Equilibrium temperature: 80°C.

[0038] 3. Solution preparation

[0039] Mixed reference substance solution preparation: Accurately weigh 250 mg of ethanol, 100 mg of dichloromethane, 150 mg of n-hexane, 250 mg of ethyl acetate, 375 mg of tetrahydrofuran, and 75 mg of toluene respectively, put the...

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Abstract

The invention relates to a method for detecting a residual solvent in an ibudilast bulk drug, which adopts a gas chromatography method, and particularly comprises the following steps: detecting six organic solvents, namely ethanol, dichloromethane, normal hexane, ethyl acetate, tetrahydrofuran and toluene by using a flame ionization detector (FID) through a programmed heating and headspace sampleinjection mode according to an external standard method. The method is simple to operate, high in sensitivity, good in accuracy and suitable for detecting the residual solvents of the six solvents andthe two solvents in the ibudilast bulk drug.

Description

technical field [0001] The invention relates to a method for detecting residual solvents in ibudilast raw material medicine. Gas chromatography is used to detect ethanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran and toluene in ibudilast according to an external standard method. It belongs to the field of drug analysis and detection. [0002] technical background [0003] Residual solvents in pharmaceuticals refer to organic volatile compounds that are used in the production of raw materials, excipients, and preparations but cannot be completely removed during the process. According to research results released by authoritative organizations such as the World Health Organization, many organic solvents are harmful to the environment and human body. When the residual solvent contained in the drug is higher than the safe value, it will not only affect the stability of the drug, but also affect the human body or the surrounding environment. Therefore, the pharmac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/68
CPCG01N30/02G01N30/06G01N30/68G01N2030/025G01N2030/062
Inventor 付丙月王金虎崔新强赵思太张宁吴伟山张云鲜婧张相军
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES