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HPLC Gradient Elution Method for Determination of Related Substances of Chlortetracycline Hydrochloride

A technology of chlortetracycline hydrochloride and related substances, applied in the field of medicine, can solve the problems such as large retention time drift, high pressure of chromatography system, insufficient stability of test solution and the like

Active Publication Date: 2022-02-22
江西省药品检验检测研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The object of the present invention is to overcome the technical problem in the method for the existing determination aureomycin hydrochloride related substance, for example avoid one or more such such as too high chromatographic system pressure, retention time drift is too big, need testing solution stability is insufficient etc. technical problem

Method used

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  • HPLC Gradient Elution Method for Determination of Related Substances of Chlortetracycline Hydrochloride
  • HPLC Gradient Elution Method for Determination of Related Substances of Chlortetracycline Hydrochloride
  • HPLC Gradient Elution Method for Determination of Related Substances of Chlortetracycline Hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0082] Embodiment 1: British Pharmacopoeia 2019 edition determines the method for aureomycin hydrochloride related substances

[0083] Solution preparation:

[0084] Test solution: dissolve 25.0 mg of test product with mobile phase B and dilute to 25.0 mL with this mobile phase;

[0085] Reference solution (a): Dissolve 25.0 mg of aureomycin hydrochloride reference substance with mobile phase B and dilute to 25.0 mL with this mobile phase;

[0086] Reference solution (b): Dilute 1.0mL of the test solution with mobile phase B to 100.0mL;

[0087] Reference solution (c): Dilute 1.0mL of reference solution (b) to 10.0mL with mobile phase B;

[0088] Reference solution (d): Dissolve 5 mg of aureomycin system suitability reference substance (which contains impurities A, B, D, E, G, H, J, K and L) with mobile phase B and dilute with this mobile phase to 5mL;

[0089] Reference solution (e): Dissolve 25.0 mg of aureomycin hydrochloride reference substance in mobile phase B and ...

Embodiment 2

[0104] Embodiment 2: HPLC gradient elution method determines aureomycin hydrochloride related substances

[0105] The chromatographic conditions for isocratic elution used in the inspection of related substances in the chlortetracycline hydrochloride species recorded in the second part of the Chinese Pharmacopoeia in the 2015 edition are: octylsilane bonded silica gel (C8 column) as filler, high chlorine Acid-dimethyl sulfoxide-water (8:525:467) (pH<2.0) is the mobile phase, the column temperature is 45°C, and the detection wavelength is 280nm.

[0106] In this example, Ultimate XB-C8 (4.6×250mm, 5μm, chromatographic column 1) and InertSustainC8 (4.6×250mm, 5μm, chromatographic column 2) were used as chromatographic columns respectively, and the hydrochloric acid prepared in Example 1 was used according to the above-mentioned Chinese Pharmacopoeia method Chlortetracycline crude drug need testing solution is measured (the retention time of first pin aureomycin is about 21.8mi...

Embodiment 3

[0107] Embodiment 3: HPLC gradient elution method determines aureomycin hydrochloride related substances

[0108] The inventor has tried four kinds of mobile phase systems in the test: 1. ammonium acetate sodium perchlorate solution (pH 2.2)-methanol, 2. 0.05mol / L dipotassium hydrogen phosphate solution (triethylamine adjusts pH to 10.0)-methanol / acetonitrile, ③perchloric acid-water-methanol-acetonitrile, ④perchloric acid-dimethyl sulfoxide-water-acetonitrile-methanol. It was found that only dimethyl sulfoxide had a good modification effect on the peak shape symmetry of the chromatographic peak of aureomycin hydrochloride. Considering that both Chinese Pharmacopoeia (2015) and BP (2019) contain a relatively high proportion of dimethyl sulfoxide in the mobile phase, and the latter adopts ultra-high performance liquid chromatography, so referring to the gradient elution method of BP (2019), we will The ratio of perchloric acid and dimethyl sulfoxide in the mobile phase is g...

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Abstract

The invention relates to a method for determining related substances of aureomycin hydrochloride by an HPLC gradient elution method. Specifically, the method for the present invention's determination of related substances in aureomycin hydrochloride or its preparations comprises the steps: (1) high performance liquid chromatography and chromatographic column are provided; (2) mobile phase is prepared; (3) test solution is prepared (4) Inject various test solutions into the liquid chromatograph respectively, measure according to the specified chromatographic conditions, record the chromatogram and calculate the content of each related substance in the test substance. The method of the present invention exhibits one or more excellent effects as described in the specification, such as low column pressure, small chromatographic peak drift and / or stable test solution.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a method for detecting the quality of medicines, in particular to a method for determining related substances of the tetracycline antibiotic chlortetracycline. The present invention uses an HPLC gradient elution method to measure the related substances of chlortetracycline hydrochloride. The method exhibits one or more aspects of superior results. Background technique [0002] Aureomycin (Chlortetracycline) is a golden yellow crystalline powder, which is produced by fermentation of Streptomyces aureofacieus. The fermentation broth is acidified and filtered to obtain a precipitate, which is dissolved in ethanol and then subjected to acid precipitation to obtain a crude product. Salt was hydrochloride crystallization. The effect and antibacterial spectrum of aureomycin are the same as those of tetracycline, its chemical formula: C22H23ClN2O8, molecular weight: 478.88, CAS registrat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/60G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/60G01N30/74G01N30/36
Inventor 刘绪平肖钦钦张银花段和祥陈希刘卫德储梅君易巧张春华
Owner 江西省药品检验检测研究院
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