Method for measuring residual solvent in tetracycline hydrochloride bulk drug by utilizing headspace gas chromatography

A technology of headspace gas chromatography and tetracycline hydrochloride, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve the problems of decreased separation effect of chromatographic columns, interference of acetone and butanol analysis, and contamination of chromatographic columns, etc., to achieve the extension of chromatographic columns The effect of long life, less interference factors and large injection volume

Active Publication Date: 2012-08-15
NINGXIA QIYUAN PHARMA
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Problems solved by technology

[0003] In "Antibiotics" 1980 03 Issue Shen Yunqing "Tetracycline Hydrochloride API Residual Solvent Limit Inspection and Determination Method-Gas Chromatography" article mentioned that residual organic solvents acetone and butanol in tetracycline hydrochloride were detected by gas chromatography. The direct sample injection method is to prepare tetracycline hydrochloride into a solution with a certain concentration, draw the solution and inject it into the gas chromatography system, tetracycline hydrochloride and residual organic solvent acetone and butanol are injected into the gas chromatography system together, because tetracycline hydrochloride is in the gas chromatograph inlet Decomposition occurs, on the one hand, it will pollute the chromatographic column, cause the separation effect of the chromatographic column to decrease, and reduce the life of the column; on the other hand, some substances in these decomposition products are detected by the detector, which interferes with the analysis of acetone and butanol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1 Chromatographic conditions:

[0026] Chromatographic column: polyethylene glycol open capillary column; column temperature: 125°C; carrier gas: nitrogen; flow rate: 3 ml / min; inlet temperature: 200°C; detector: FID; detector temperature: 250°C; hydrogen Flow: 30 ml / min; air flow: 400 ml / min.

[0027] 2 Headspace conditions:

[0028] Headspace vial heating temperature: 80°C; headspace heating time: 25min; quantitative loop temperature: 105°C; transfer tube temperature: 125°C; quantitative loop volume: 1ml.

[0029] 3 Solution preparation:

[0030] (1) n-butanol stock solution: Accurately draw 1ml of n-butanol, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute it with water to the mark, and shake well.

[0031] (2) Acetone stock solution: Accurately absorb 1ml of acetone, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute to the mark with wat...

Embodiment 2

[0042] 1 Chromatographic conditions:

[0043] Chromatographic column: polyethylene glycol open capillary column; column temperature: 125°C; carrier gas: nitrogen; flow rate: 3 ml / min; inlet temperature: 200°C; detector: FID; detector temperature: 250°C; hydrogen Flow: 30 ml / min; air flow: 400 ml / min.

[0044] 2 Headspace conditions:

[0045] Headspace vial heating temperature: 80°C; headspace heating time: 25min; quantitative loop temperature: 105°C; transfer tube temperature: 125°C; quantitative loop volume: 1ml.

[0046] 3 Solution preparation:

[0047] (1) n-butanol stock solution: Accurately draw 1ml of n-butanol, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute it with water to the mark, and shake well.

[0048] (2) Acetone stock solution: Accurately absorb 1ml of acetone, put it in a 200ml volumetric flask filled with a small amount of water in advance, dissolve it completely, dilute to the mark with wat...

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Abstract

The invention relates to a method for measuring a residual solvent in a tetracycline hydrochloride bulk drug by utilizing headspace gas chromatography. The method comprises the following steps of: preparing tetracycline hydrochloride into a solution and placing the solution into a headspace bottle; heating the solution, and volatilizing a volatile organic solvent from the solution; after balance is achieved, taking a gas at the upper part in the headspace bottle, and injecting the gas into a gas chromatograph for separation and measurement. The method for measuring the residual solvent in the tetracycline hydrochloride bulk drug by utilizing headspace gas chromatography can prevent solid tetracycline hydrochloride from remaining at an injection port of a gas chromatographic column, the chromatographic column can not be affected, thus the service life of the chromatographic column is prolonged, also the interference factors are less, the measured result is accurate, and the detection limit is high because of great sample size.

Description

technical field [0001] The invention belongs to the technical field of detection of biological raw materials, and in particular relates to a method for determining residual solvents in tetracycline hydrochloride raw materials by headspace gas chromatography. Background technique [0002] Residual solvents in pharmaceuticals refer to organic solvents that cannot be completely removed during the production of raw materials or excipients, as well as during the preparation of preparations. Organic solvents are harmful to the human body, so in the 2010 edition of the Pharmacopoeia of the People's Republic of China, the second appendix P has certain requirements on its limit, but there is no specific regulation on the determination method. [0003] In "Antibiotics" 1980 03 Issue Shen Yunqing "Tetracycline Hydrochloride API Residual Solvent Limit Inspection and Determination Method-Gas Chromatography" article mentioned that the residual organic solvents acetone and butanol in te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/14G01N30/12G01N30/02
Inventor 李学兵邹学锋
Owner NINGXIA QIYUAN PHARMA
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