Method for determining content of chlortetracycline premix and related substances

A related substance, chlortetracycline technology, applied in the field of analysis and testing, can solve the problems of the influence of content test accuracy, low work efficiency, and low production efficiency, and achieve the goal of improving detection speed and accuracy, reducing inspection cost, and improving detection efficiency Effect

Inactive Publication Date: 2018-02-23
金河生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Practice has shown that the use of microbial methods to determine the content has several disadvantages: 1) the method is cumbersome and takes a long time, resulting in low work efficiency; 2) the method has many influencing factors, which have a greater impact on the accuracy of the content t

Method used

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  • Method for determining content of chlortetracycline premix and related substances
  • Method for determining content of chlortetracycline premix and related substances
  • Method for determining content of chlortetracycline premix and related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] repeatability test

[0060] Get the chlortetracycline test solution of the above-mentioned configuration, inject Shimadzu LC-2040 type ultra-high performance liquid chromatography, carry out high-performance liquid chromatography analysis according to the above-mentioned chromatographic conditions, carry out 6 parallel determinations continuously, and record 6 parallel determinations The peak area of ​​each component, the results are shown in Table 1, wherein the high performance liquid chromatogram of parallel test group 2 is as follows figure 1 shown.

[0061] Table 1 repeatability (system precision) test data statistical table

[0062]

[0063]

[0064] As can be seen from Table 1, the same chlortetracycline need testing solution is measured for 6 consecutive injections, the peak area RSD of chlortetracycline is 0.11%, the peak area RSD of tetracycline is 0.26%, and the RSD of peak area of ​​tetracycline is 1.7%. The peak area RSD of chlortetracycline was 0.4...

Embodiment 2

[0066] Reproducibility test

[0067] Reproducibility, also known as method precision, is determined by testing the same sample on different days with different instruments by different inspectors.

[0068] Get the aureomycin working standard solution of above-mentioned configuration, inject Shimadzu LC-2040 type ultra-high performance liquid chromatograph, carry out high performance liquid chromatography analysis according to above-mentioned chromatographic conditions, obtain aureomycin working standard solution high performance liquid chromatography, Such as figure 2 shown, yes figure 2 The analysis shows that the peak area of ​​aureomycin in the figure is 2424882.

[0069] Take the aureomycin test solution of the above-mentioned configuration, and measure it 6 times by two inspectors on different dates respectively, through the formula: aureomycin in aureomycin premix or aureomycin Carry out the calculation, and record the calculation result, statistically analyze the ...

Embodiment 3

[0075] accuracy test

[0076] Accuracy is the closeness between the measured value and the true value, and the accuracy of the method is usually expressed by the recovery rate. Select a chlortetracycline premix sample of a known specification (the chlortetracycline content is 20.2wt%, tetracycline 1.2wt%, epitrope chlortetracycline 0.51wt%, 2-acetyl-2-decarboxamidotetracycline 0.47 wt%, 2-acetyl-2-descarboxamidomycin 0.22wt%, epitetracycline and demethylchlortetracycline are all less than 0.1wt%), diluted with 0.01mol / L HCl, and prepared three concentration levels Chlortetracycline premix sample solution, 3 parts of each grade parallel determination, carry out 9 times of measurement altogether, then combine the peak area of ​​aureomycin in the working standard solution chromatogram that obtains Chlortetracycline in the embodiment 2, by formula gold Aureomycin and Calculate the content of aureomycin and related substances in each group, and then calculate the recovery rate...

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Abstract

The invention relates to a method for determining the content of a chlortetracycline premix and related substances and belongs to the technical field of analysis and testing. The method adopts the following chromatographic conditions: a C18 chromatographic column, a column temperature of 45 DEG C, detection wavelength of 280 nm, a mobile phase which is a mixed solution of water, a phosphoric acidsolution and N, N-dimethylformamide in a volume ratio of 220: 80: 100, the concentration of the phosphoric acid solution of 2 mol/L, a pump flow rate of 0.4 mL/min, an injection volume of 4 microliters and running time of 5min. The method comprises preparing a chlortetracycline standard stock solution, a chlortetracycline work standard solution and a chlortetracycline test solution and carrying out high performance liquid chromatography analysis so that relevant substance content contents are calculated through a main component self-control method through a peak area external standard method.The method has good repeatability, good reproducibility, high accuracy, a wide linear test range and good durability, saves the use amounts of all solutions and improves the detection speed and precision.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, in particular to a method for measuring the content of aureomycin premix and related substances. Background technique [0002] As a feed additive, aureomycin premix is ​​a chlortetracycline calcium salt made from the whole fermentation broth of aureomycin-producing bacteria and an appropriate amount of calcium carbonate. The active ingredient is mainly aureomycin, but it also contains some Related fermentation by-products, such as tetracycline, epitetracycline, epiclotetracycline, demethylaureomycin, 2-acetyl-2-deformamidotetracycline, 2-acetyl-2-deformamidotetracycline, etc. . In the national veterinary drug standard, the content of aureomycin is determined by microbiological assay method, and there is no requirement for the detection and control of related substances. Practice has shown that the use of microbial methods to determine the content has several disadvantages: 1) the m...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 谢昌贤秦定宇金玲玲杨晓亚刘运添云喜报王鹏飞
Owner 金河生物科技股份有限公司
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