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Method for determining content of phenoxyacetic acid in phenoxyacetic acid tested sample

A technology based on phenoxyacetic acid and phenoxyacetic acid, applied in the field of chemical analysis, can solve problems such as poor accuracy, high toxicity of reagents, and susceptibility to impurities

Pending Publication Date: 2021-05-18
NORTH CHINA PHARMA COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of this, the present invention provides a method for determining the content of phenoxyacetic acid in the tested sample of phenoxyacetic acid, so as to solve the problems of high reagent toxicity, easy to be affected by impurities and poor accuracy in the existing method

Method used

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  • Method for determining content of phenoxyacetic acid in phenoxyacetic acid tested sample
  • Method for determining content of phenoxyacetic acid in phenoxyacetic acid tested sample

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preparation example Construction

[0031] (a) Preparation of reference substance solution: Accurately weigh the phenoxyacetic acid standard substance, add mobile phase to dissolve, and quantitatively dilute to make the concentration Ca 1 (0.02~0.5mg / mL) phenoxyacetic acid standard reference solution, shake well, and dilute to volume;

[0032] (b) Preparation of the tested sample solution: Accurately weigh the phenoxyacetic acid sample, add mobile phase to dissolve, and quantitatively dilute to make a phenoxyacetic acid tested sample solution with a concentration of Ca (0.02-0.5 mg / mL), shake well ,Volume;

[0033] (c) Chromatographic conditions: Octadecylsilane bonded silica gel is used as a filler, and a mixed solution of water, methanol, and pH 3.5 phosphate aqueous solution with a volume ratio of 100:80:20 is used as a mobile phase, and the flow rate is 1.4mL / min; the detection wavelength is 220nm; the column temperature is 25°C; the number of theoretical plates should not be less than 2000 based on the ma...

Embodiment 1

[0041] Chromatographic conditions: using Elite C 18 The reverse phase column is 4.6mm×150mm, 5μm; the mobile phase is a mixed solution of water, methanol and pH3.5 phosphate aqueous solution with a volume ratio of 100:80:20; the flow rates are 1.0mL / min, 1.4mL / min and 2.0mL / min; UV detector, the detection wavelength is 292nm; column temperature is 25°C (room temperature); the number of theoretical plates should not be less than 2000 based on the main peak.

[0042] Sample solution to be tested: Accurately weigh the phenoxyacetic acid sample, add mobile phase to dissolve and quantitatively dilute to make a solution containing 0.02mg of phenoxyacetic acid sample per 1mL, shake well, and constant volume;

[0043] Reference substance solution: Accurately weigh the phenoxyacetic acid standard, add mobile phase to dissolve, and quantitatively dilute to make a solution of 0.02mg phenoxyacetic acid standard in every 1mL, shake well, and constant volume;

[0044] Determination method:...

Embodiment 2

[0052] The chromatographic conditions are the same as in Example 1.

[0053] Sample solution to be tested: Accurately weigh the phenoxyacetic acid sample, add mobile phase to dissolve and quantitatively dilute to make a solution containing 0.2mg of phenoxyacetic acid sample per 1mL, shake well, and constant volume;

[0054] Reference substance solution: Accurately weigh the phenoxyacetic acid standard, add mobile phase to dissolve, and quantitatively dilute to make a solution containing 0.2mg of phenoxyacetic acid standard per 1mL, shake well, and constant volume;

[0055] Determination method and the step of calculating phenoxyacetic acid content are identical with embodiment 1, and the chromatogram of phenoxyacetic acid standard substance and phenoxyacetic acid sample is as follows Figure 1~2 As shown, the contents of phenoxyacetic acid in the calculated samples were 96.7%, 98.2% and 96.8%, respectively.

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Abstract

The invention discloses a method for determining the content of phenoxyacetic acid in a phenoxyacetic acid sample to be detected, and belongs to the field of chemical analysis. High performance liquid chromatography is adopted to determine the content of phenoxyacetic acid. The method comprises the following steps of: (a) preparing a reference substance solution; (b) preparing a to-be-detected sample solution; (c) setting chromatographic conditions, specifically, adopting octadecylsilane chemically bonded silica as a filler, weighing 68g of potassium dihydrogen phosphate, adding purified water until the volume achieves 1000ml, adjusting the pH value by using phosphoric acid to 3.5 so as to obtain pH 3.5 phosphate, setting the ratio of water to methanol to the pH 3.5 phosphate in a mobile phase to be 100: 80: 20, setting the wavelength to be 220nm, and setting the flow velocity to be 1.4; and (d) performing a determination method, specifically, precisely measuring 10 [mu] L of the to-be-detected sample solution and 10 [mu] L of the reference substance solution separately, injecting the solutions into a liquid chromatograph, recording chromatograms of the to-be-detected sample and the reference substance, and performing calculation by peak areas according to an external standard method to obtain the content of the to-be-detected phenoxyacetic acid sample. The method has the advantages of simple and convenient operation process, high precision and good stability, and can effectively eliminate the influence of a titration method on a determination result.

Description

technical field [0001] The invention relates to a method for determining effective components in antibiotic raw materials, in particular to a method for determining the content of phenoxyacetic acid in a phenoxyacetic acid test sample, and belongs to the field of chemical analysis. Background technique [0002] Phenoxyacetic acid, white needle crystal. 1g product is soluble in about 75ml water, easily soluble in ethanol, ether, benzene, carbon disulfide and glacial acetic acid. The melting point is 98°C. The boiling point is 285°C (partially decomposed), used as the raw material for penicillin V potassium, and its structural formula is as follows: [0003] [0004] At present, the detection method of phenoxyacetic acid content in domestic enterprises is titration method, but this method is complicated to operate and has poor accuracy. [0005] Existing literature (China Pharmaceutical Industry, 2004, 13 (5), 38) has reported the content of phenoxyacetic acid in the det...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/32G01N30/34G01N30/36G01N30/54G01N30/86
CPCG01N30/02G01N30/06G01N30/32G01N30/34G01N30/36G01N30/54G01N30/86G01N2030/324G01N2030/047
Inventor 张军立段志钢马金玉刘倩王新辉穆军明崔克娇赵彬杨婷程璐英曹欢翟梦师书迪刘磊赵汝梅宋斌
Owner NORTH CHINA PHARMA COMPANY
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