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Method for detecting content of oxytetracycline hydrochloride

A technology of oxytetracycline hydrochloride and detection method, which can be applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as impurity and complicated operation, and achieve the effects of high recovery rate, simple operation, good stability and repeatability

Active Publication Date: 2020-02-07
JIANGXI GUOYAO PHARMA LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing detection method for the content of oxytetracycline hydrochloride is complicated to operate, and the pH is adjusted many times, and the peak purity factor is less than 990, and the peak is not pure.
At present, there is no simple and effective HPLC detection method for oxytetracycline hydrochloride. In order to facilitate the synthesis personnel to analyze the yield, the present invention studies the HPLC analysis method and screens out a simple, fast and accurate method for measuring the content of oxytetracycline hydrochloride.

Method used

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  • Method for detecting content of oxytetracycline hydrochloride
  • Method for detecting content of oxytetracycline hydrochloride
  • Method for detecting content of oxytetracycline hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1: use the method for high-performance liquid chromatography detection oxytetracycline hydrochloride content

[0044] Take 100mL of purified water, add 5.23g of dipotassium hydrogen phosphate, dissolve and add sodium hydroxide to adjust the pH to 8.0.

[0045] Take 400mL of purified water, add 120g of tert-butanol, after dissolving, add 100ml of the above-mentioned dipotassium hydrogen phosphate solution, mix well, and filter to obtain the mobile phase;

[0046] Take 1000mL of purified water, add 4.5mL of concentrated hydrochloric acid, mix well, and prepare a diluted solution;

[0047] Take about 44mg of oxytetracycline hydrochloride, accurately weigh it, put it in a 100ml measuring bottle, add 0.05mol / L hydrochloric acid solution to dissolve and dilute to the mark, shake well, accurately measure 5ml, put it in a 10ml measuring bottle, add 0.05mol / L The hydrochloric acid solution is diluted to the mark, shakes up, makes need testing solution;

[0048] Take...

Embodiment 2

[0051] Embodiment 2: Dipotassium hydrogen phosphate solution and tert-butanol ratio investigation

[0052]Three mobile phases with volume ratios of 10:90, 20:80, and 30:70 were prepared by using the solution containing 0.3 mol / L dipotassium hydrogen phosphate and tert-butanol prepared according to Example 1. The rest of the conditions are the same as in Example 1, and the resolution, main peak retention time and impurity peak quantity of different mobile phases are shown in Table 1.

[0053] Table 1 The resolution, main peak retention time and impurity peak quantity of different mobile phase ratios

[0054]

[0055] It can be seen that, with the reduction of tert-butanol in the mobile phase, the retention time of the main peak is prolonged, and the separation degree of the main peak and adjacent impurities is the best when the ratio of dipotassium hydrogen phosphate solution and tert-butanol is 20:80 Good, and the retention time of the main peak is moderate compared to the...

Embodiment 3

[0056] Embodiment 3: the investigation to dipotassium hydrogen phosphate solution concentration

[0057] Take 100mL of purified water, add 0.1mol (1.74g), 0.2mol (3.48g), 0.3mol (5.23g) and 0.4mol (6.97g) of dipotassium hydrogen phosphate, dissolve and add sodium hydroxide to adjust the pH to 8.0, take 100ml of the above solution was mixed with 400ml of tert-butanol solution (concentration: 0.3g / mL), filtered, and four mobile phases were prepared respectively. All the other conditions are the same as in Example 1. The resolution, retention time of main peak and number of impurity peaks of different mobile phases are shown in Table 2.

[0058] Table 2 The degree of separation and the retention time of the main peak and the number of impurity peaks of different concentrations of dipotassium hydrogen phosphate solution

[0059]

[0060]

[0061] As the concentration of dipotassium hydrogen phosphate increases, the retention time of the main peak is relatively advanced, an...

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Abstract

The invention relates to a method for detecting the content of oxytetracycline hydrochloride. The method comprises the following steps: preparing a test solution and a reference solution, and then respectively injecting the test solution and the reference solution into a high performance liquid chromatograph for detection, wherein the test solution is prepared by dissolving a sample in a 0.05mol / Lhydrochloric acid solution and filtering the solution with a microfiltration membrane, the chromatographic conditions are as follows: the mobile phase is 0.3mol / L dipotassium phosphate (the pH is adjusted to 8.0 by sodium hydroxide)-0.3g / mL tertiary butanol solution (20:80), the chromatographic column is 4.6mm * 250mm packed with a 10 mu m spherical styrene divinylbenzene copolymer packed column,the detection wavelength is 254nm, the flow rate is 1.2ml / min, and the column temperature is 60 DEG C. By adopting the method provided by the invention, the appearance time of the main peak is shortened, the degree of separation is good, the method is simple to operate, high in precision, high in recovery rate and good in stability and repeatability, and after continuous analysis of multiple samples on the chromatographic column, the column pressure and the number of theoretical plates of the main peak do not change significantly.

Description

technical field [0001] The invention belongs to a drug detection method, in particular to a detection method for the content of a tetracycline antibiotic oxytetracycline hydrochloride crude drug. Background technique [0002] Oxytetracycline hydrochloride, also known as oxytetracycline hydrochloride and oxytetracycline hydrochloride, has the following structural formula: [0003] [0004] It is a tetracycline antibiotic discovered in the late 1940s. Oxytetracycline is a broad-spectrum antibiotic produced by the metabolism of Streptomyces fissures. It has the characteristics of broad antibacterial spectrum and high efficacy. All have good inhibitory effects. Oxytetracycline was discovered by Finlay et al. in 1950 in Streptomyces fissures isolated near the Pfizer laboratory. In 1953, biochemist Robert B Woodward analyzed the structure of oxytetracycline, which enabled mass production and sales of oxytetracycline. Oxytetracycline hydrochloride can be used to treat rickett...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/34G01N30/06
CPCG01N30/88G01N30/34G01N30/06G01N2030/047G01N2030/884
Inventor 庄庄万义斌葛友群左飞鸿杨明詹业奇艾嘉浩钟佩敏吴鑫王建涛李可晔刘绥阳
Owner JIANGXI GUOYAO PHARMA LLC
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