Measuring method of mesoxalic acid in tetracycline filter liquor

A determination method and technology for oxalic acid, applied in the field of medical testing, can solve the problems of inability to quickly detect oxalic acid content, increase the difficulty of environmental protection treatment, and take a long time in headspace operation, and achieve the improvement of working efficiency of recovery operators, low cost, and improved use. The effect of efficiency

Active Publication Date: 2013-10-02
NINGXIA QIYUAN PHARMA
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

If such a large amount of oxalic acid is treated with waste liquid, it has the following disadvantages: ① Increase the difficulty of environmental protection treatment; ② Increase production costs; ③ Third, waste of resources
However, the headspace operation of this method takes a long time and cannot quickly detect the content of oxalic acid in tetracycline acidification waste liquid.

Method used

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  • Measuring method of mesoxalic acid in tetracycline filter liquor
  • Measuring method of mesoxalic acid in tetracycline filter liquor
  • Measuring method of mesoxalic acid in tetracycline filter liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1 Chromatographic conditions:

[0028] Chromatographic column: C18 column, Agilent XDB, 150mm×4.6mm; mobile phase: 0.15% tetrabutylammonium bisulfate (adjust pH to 7.4 with ammonia water); mobile phase flow rate: 0.8ml / min; detection wavelength: 210nm.

[0029] 2 Preparation of sample solution: Dilute the tetracycline filtrate with water until the concentration of oxalic acid is 0.1mg / ml~2mg / ml. At the same time, 0.15 g of the oxalic acid reference substance was accurately weighed and placed in a 100 ml measuring bottle, dissolved in water and diluted to the mark as a reference solution.

[0030] 3 Determination: inject the solution into the high performance liquid chromatograph, record the chromatogram and analyze it (the chromatogram is figure 1 ).

[0031] The content of oxalic acid in the sample solution was determined to be 3.52%.

Embodiment 2

[0033] 1 Chromatographic conditions:

[0034] Chromatographic column: C18 column, Agilent XDB, 150mm×4.6mm; mobile phase: 0.2% tetrabutylammonium bisulfate (adjust pH to 7.5 with ammonia water); mobile phase flow rate: 1.0ml / min; detection wavelength: 215nm.

[0035] 2 Preparation of sample solution: Dilute the tetracycline filtrate with water until the concentration of oxalic acid is 0.1mg / ml~2mg / ml. At the same time, 0.15 g of the oxalic acid reference substance was accurately weighed and placed in a 100 ml measuring bottle, dissolved in water and diluted to the mark as a reference solution.

[0036] 3 Determination: inject the solution into the high performance liquid chromatograph, record the chromatogram and analyze it (the chromatogram is figure 2 ). The content of oxalic acid in the sample solution was determined to be 3.58%.

Embodiment 3

[0038] 1 Chromatographic conditions:

[0039] Chromatographic column: C18 column, Agilent XDB, 150mm×4.6mm; mobile phase: 0.1% tetrabutylammonium bisulfate (adjust pH to 7.3 with ammonia water); mobile phase flow rate: 1.2ml / min; detection wavelength: 205nm.

[0040] 2 Preparation of sample solution: Dilute the tetracycline filtrate with water until the concentration of oxalic acid is 0.1mg / ml~2mg / ml. At the same time, 0.15 g of the oxalic acid reference substance was accurately weighed and placed in a 100 ml measuring bottle, dissolved in water and diluted to the mark as a reference solution.

[0041] 3 Determination: inject the solution into the high performance liquid chromatograph, record the chromatogram and analyze it (the chromatogram is image 3 ). The content of oxalic acid in the sample solution was determined to be 3.72%.

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Abstract

The invention relates to a measuring method of mesoxalic acid in tetracycline filter liquor. The measuring method adopts high efficiency liquid chromatography, and the high efficiency liquid chromatography determines to take a C18 column as a chromatographic column, 0.1%-0.2% of tetrabutylammonium hydrogen sulfate as a mobile phase and 0.7-1.2 ml / minute flow velocity of the mobile phase and 205-220 nanometer detection wavelength as chromatographic conditions. The measuring method disclosed by the invention has the advantages of accuracy and reliability in detection result, fast analysis, less interference factor, easiness for preparation, low cost, easiness for operation, and the like.

Description

technical field [0001] The invention relates to the technical field of medical detection, in particular to a method for determining oxalic acid in tetracycline filtrate. Background technique [0002] The production of antibiotics by microbial fermentation technology is the main technology of antibiotic production at present. The method is characterized by large output, low cost and easy scale production. Tetracycline is produced by Streptococcus aureus through microbial fermentation, acidification, crystallization and refining. During the fermentation process, tetracycline exists in the microbial cells and needs to be acidified to release tetracycline from the cells. Among the acidic substances that can be used for tetracycline acidification, oxalic acid is widely used due to its moderate acidity, low cost and high acidification release rate. [0003] During the tetracycline acidification process, the amount of oxalic acid added was 3.6% of the volume of the fermentati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 邹学锋孙瑞君
Owner NINGXIA QIYUAN PHARMA
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