Liquid chromatography method for simultaneously determining contents of procaine, penicillin and streptomycin

A liquid chromatographic analysis and procaine technology, which can be used in measurement devices, analytical materials, material separation, etc., can solve the problems of inaccurate detection and long detection time of detection methods, and achieve strong specificity, high accuracy, high precision effect

Inactive Publication Date: 2018-04-06
CHONGQING FANGTONG ANIMAL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] For the above-mentioned deficiencies that exist in the prior art, the object of the present invention is to provide a kind of liquid chromatographic analys

Method used

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  • Liquid chromatography method for simultaneously determining contents of procaine, penicillin and streptomycin
  • Liquid chromatography method for simultaneously determining contents of procaine, penicillin and streptomycin
  • Liquid chromatography method for simultaneously determining contents of procaine, penicillin and streptomycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Through this implementation to determine the content of procaine, penicillin and streptomycin, and verify their specificity.

[0033] 1. The detection conditions are as follows:

[0034] Chromatographic column: Octadecylsilane bonded silica gel as filler (C18 250mm×4.6, μm);

[0035] Mobile phase: mixed buffer - acetonitrile (88:12) (see quality standard for detailed preparation method);

[0036] Flow rate: 1.0mL / min;

[0037] Injection volume: 20μL;

[0038] Detection wavelength: 205nm;

[0039] Column temperature: 40°C;

[0040] 2. The control solution is as follows:

[0041] Penicillin reference substance solution (hereinafter referred to as liquid a): appropriate amount of penicillin reference substance is dissolved in mobile phase to make 2mg·mL -1 Reference substance solution.

[0042] Streptomycin reference substance solution (hereinafter referred to as liquid b): appropriate amount of streptomycin reference substance was dissolved in mobile phase to make ...

Embodiment 2

[0050] Using the detection conditions, control solution and measurement method in Example 1, the single component linear relationship investigation experiment was carried out.

[0051] 1. Penicillin linear relationship

[0052] Accurately draw appropriate amount of solution a, add mobile phase to make penicillin containing 0.2, 0.4, 0.6, 1.0, 2.0 mg·mL respectively -1The reference substance solution is measured by the chromatographic conditions under the assay item, and the regression analysis is carried out with the peak area (A) to the concentration (C), as shown in Table 2, figure 2 shown.

[0053] Table 2 penicillin linear relationship results

[0054]

[0055] It can be seen that the concentration of penicillin is in the range of 0.26016---2.6016 mg / mL, and there is a good linear relationship, and the correlation coefficient r=0.9999.

[0056] 2. Streptomycin linear relationship

[0057] Precisely draw appropriate amount of solution b, add mobile phase to make str...

Embodiment 3

[0067] Using the detection conditions, contrast solution and assay method in Example 1, examine the accuracy, stability and precision on the basis of implementing 1 and 2.

[0068] 1. Accuracy

[0069] Sample addition recovery rate test: Accurately measure 9 parts of the test solution with known content of each component, each 3 parts is a group, and each group is added with 1 mL, 3 mL and 5 mL of the control solution according to the three concentrations of low, medium and high respectively, shake Evenly, dilute to the scale line, accurately measure 20 μ L decibels and inject into the chromatograph, record the chromatogram, and calculate the average recovery rate and RSD of procaine, penicillin, and streptomycin. The results are shown in Table 4. From Table 4, the three The average sample recovery rate of each component is greater than 97%, and the RSD is less than 2.0%, indicating that the accuracy of the present invention is high.

[0070] Table 4 Accuracy inspection resul...

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Abstract

The invention discloses a liquid chromatography method for simultaneously determining the contents of procaine, penicillin and streptomycin. The method includes the steps of first separately preparingstandard solutions of procaine, penicillin and streptomycin control components, then preparing a test solution containing procaine, penicillin and/or streptomycin components, using the liquid chromatograms obtained by liquid chromatography to draw the standard curves of procaine, penicillin and streptomycin, and finally testing the test solution and using the standard curves of procaine, penicillin and streptomycin to calculate the contents of procaine, penicillin and/or streptomycin. The method can accurately detect the contents of procaine, penicillin and streptomycin, has the advantages ofstrong specificity, high precision, good stability and high accuracy, is suitable for the quality control of procaine penicillin-streptomycin unilateral and compound products in the veterinary drug industry, and can effectively save the testing cost and time.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a liquid chromatography analysis method for simultaneously determining the contents of procaine, penicillin and streptomycin. Background technique [0002] At present, the United States Pharmacopoeia has included the quality standard of "Procaine Penicillin-Dihydrostreptomycin Sulfate Injection". The method is not perfect, the selectivity is poor, and there are many interference factors. There is no standard method for the content determination of penicillin compound preparations in China. The iodometric method is based on the principle of oxidation-reduction titration, which requires a faster completion of the titration process. If the antioxidant or other auxiliary materials used in the formula can interfere with the titration process and results, the grasp of the time point of adding the starch indicator solution can increase. Large errors in titration results. ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 毕海林苏玲肖裕章张超袁启峰
Owner CHONGQING FANGTONG ANIMAL PHARMA
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