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Pyrazolone effective constituent detection method

A technology of active ingredients and detection methods, which is applied in the field of detection of active ingredients of pyrazolones, can solve the problems of long analysis time, high analysis value, and difficulty in judging the end point, and achieves the effects of accurate measurement results and simple operation.

Pending Publication Date: 2020-02-25
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this detection method, because of the nitrosation reaction, the reaction temperature needs to be controlled, resulting in a large workload. At the same time, starch-potassium iodide test paper is used as an indicator, and there is a false end point. The end point is not easy to judge, and the detection parallelism is poor. In addition, during the reaction NO - Due to the steric hindrance effect, only 1mol substitution occurs, but in the actual reaction, there are two hydrogen substitutions, resulting in deviations in the measurement results
Zhang Lijie etc. have disclosed a kind of high-performance liquid chromatography quantitative determination 1, the method for 3-dimethyl-5-pyrazolone, by adopting high-performance liquid chromatography quantitative determination DP (being 1,3-dimethyl-5 -pyrazolone), this method has good sensitivity, recovery and repeatability, but there are many factors affecting high performance liquid chromatography, including mobile phase, detection wavelength, flow rate, column temperature, fixation, etc., resulting in relatively low analysis cost. High cost, long analysis time, and expensive liquid chromatograph and routine maintenance also limit the application of this method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Sample 1 (the content of p-mepizolon is 97.52%, and the relative molecular mass of p-mepizolon is 188.2)

[0053] The detection method is:

[0054](1) Take sample 1 with a weight of 0.3000g in a container, add 20ml of distilled water to disperse, then add a sodium carbonate solution with a concentration of 1.2mol / l, so that the mass ratio of sodium carbonate to the sample is 3:5, and stir for 20min. If it is fully dissolved, a dissolved solution is obtained;

[0055] (2) Add 0.6% sodium bicarbonate solution to the dissolving solution in step (1), the mass ratio of sodium bicarbonate to the sample to be tested is 3:1, and continue to stir for 2min to obtain a mixed solution;

[0056] (3) add 10g / L starch indicator in mixed solution, and use the iodine standard solution titration of 0.03mol / l, be titration end point when solution turns light brown, the volume that this moment consumes iodine standard solution is 175ml;

[0057] (4) Carry out blank test in the same way, ...

Embodiment 2

[0060] Sample 2 (the content of pyrazolone p-sulfonic acid is 99.36%, and the relative molecular mass of p-mepyrazolone is 254.3)

[0061] The detection method is:

[0062] (1) Take sample 1 with a weight of 0.5000g in a container, add 20ml of distilled water to disperse, then add a sodium carbonate solution with a concentration of 0.8mol / l, so that the mass ratio of sodium carbonate to the sample to be tested is 53:100, stir 15 minutes to make it fully dissolved, to obtain a dissolved solution;

[0063] (2) Add 0.6% sodium bicarbonate solution to the dissolving solution in step (1), the mass ratio of sodium bicarbonate to the sample to be tested is 1:1, and continue to stir for 4min to obtain a mixed solution;

[0064] (3) add 12g / L starch indicator in mixed solution, and use the iodine standard solution titration of 0.05mol / l, be titration end point when solution turns light brown, the volume that this moment consumes iodine standard solution is 52ml;

[0065] (4) Carry ou...

Embodiment 3

[0068] Sample 3 (the content of phenylpyrazolone is 98.62%, and the relative molecular mass of p-methylpyrazolone is 174.2)

[0069] The detection method is:

[0070] (1) Weigh sample 1 with a weight of 1.0000g in a container, add 20ml of distilled water to disperse, then add a sodium carbonate solution with a concentration of 1mol / l, so that the mass ratio of sodium carbonate to the sample to be tested is 58:100, and stir for 10min Make it fully dissolved to obtain a dissolved solution;

[0071] (2) Add 0.6% sodium bicarbonate solution to the dissolving solution in step (1), the mass ratio of sodium bicarbonate to the sample to be tested is 3:1, and continue stirring for 5min to obtain a mixed solution;

[0072] (3) Add 8g / L starch indicator in mixed solution, and use the iodine standard solution titration of 0.06mol / l, be the titration end point when solution turns light brown, the volume that this moment consumes iodine standard solution is 96ml;

[0073] (4) Carry out bl...

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Abstract

The invention belongs to the field of compound detection, and specifically discloses a pyrazolone effective constituent detection method. The detection method is used for detecting pyrazolones effective constituents in a reaction system through an iodine substitution reaction method, and the detection method comprises to-be-detected sample dissolution, titration and blank correction. In a titration process, substitution of two hydrogen positions happens on a benzene ring of the to-be-detected sample when titrating solution reacts with the to-be-detected sample, and appearance of a false end point is avoided, thus, a detection result can be more accurate, meanwhile, the detection method is simple to operate and has no high requirement on detection equipment and detection environment.

Description

technical field [0001] The invention belongs to the field of compound detection, and in particular relates to a method for detecting active ingredients of pyrazolone. Background technique [0002] Pyrazolones are important intermediates for the synthesis of medicines, pesticides bafenex, herbicides pyrazolid and dyes, etc. They are widely used. Real-time detection of the content of pyrazolone active ingredients in the production process is very important for tracking the reaction process and controlling the product. The quality is of great significance, but there are few reports on the determination method of pyrazolone at present. The method widely used at present is the nitrosation method. Since pyrazolone and sodium nitrite standard titration solution undergo nitrosation reaction under acidic conditions, the pyrazolone in the pyrazolone sample can be measured by using starch-potassium iodide test paper to check the end point. Ketone Active Ingredients. However, in this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/78
CPCG01N31/16G01N21/78
Inventor 陈安源罗芳杨伦花张美艳郑越晴王舒萍
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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