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Liquid chromatographic analysis method for determining content of oxolinic acid

A liquid chromatography analysis, oxolinic acid technology, applied in the direction of measuring devices, analysis materials, material separation, etc., can solve the problems of small measurement range, high measurement results, unsatisfactory, etc., to achieve simple measurement methods, high sensitivity, exclusive good sex effect

Active Publication Date: 2014-03-19
MASTEAM BIO TECH
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  • Claims
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AI Technical Summary

Problems solved by technology

[0003] In the currently implemented quality standards for imported veterinary drugs and the European Pharmacopoeia, the determination of the content of oxquinic acid is carried out by non-aqueous titration method. Because the oxolinic acid prepared by the chemical synthesis method contains a small amount of acidic impurities, it will interfere with the display of the acid-base indicator. color, and the presence of acidic impurities will cause the measurement results to be higher than the actual
[0004] In addition, although some methods using liquid chromatography to measure the content of oxolinic acid have been disclosed in the existing literature, their measurement range is small, suitable for the measurement of low-level oxolinic acid, and not suitable for measuring the oxolinic acid prepared by chemical synthesis. Quantitic acid product content and measurement results are not satisfactory

Method used

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Embodiment 1

[0026] A chromatographic column using octadecyl bonded silica gel as the stationary phase, column length 150mm x inner diameter 4.6mm x packing particle size 5μm, mobile phase is acetonitrile: tetrahydrofuran (containing 0.03% tri-n-octylamine in the total volume of the mobile phase): Water (containing 0.3% citric acid in the total volume of the mobile phase) = 20:10:70, the flow rate is 0.5mL / min, the detection wavelength is 330nm, the column temperature is 40°C, and the injection volume is 10μL. Accurately weigh 20mg of oxolinic acid sample (batch number 130801) and reference substance respectively, add appropriate amount of mixed solvent of dimethylformamide and methanol (volume ratio: 2:3) to a 100mL volumetric flask, and dissolve in a water bath at 80°C After that, add the above-mentioned mixed solvent of dimethylformamide and methanol to dilute to the mark, and filter with a 0.45 μm microporous membrane before sample injection for chromatographic analysis.

[0027] Get a...

Embodiment 2

[0029] A chromatographic column using octadecyl bonded silica gel as the stationary phase, column length 150mm x inner diameter 4.6mm x packing particle size 10μm, mobile phase is acetonitrile: tetrahydrofuran (containing 0.04% tri-n-octylamine in the total volume of the mobile phase): Water (containing 0.3% citric acid in the total volume of the mobile phase) = 20:10:70, the flow rate is 0.45mL / min, the detection wavelength is 320nm, the column temperature is 35°C, and the injection volume is 10μL. Accurately weigh 20mg of oxolinic acid sample (batch number 130802) and the reference substance respectively, put into a 100mL volumetric flask, add an appropriate amount of mixed solvent of dimethylformamide and methanol (volume ratio: 2:3), and dissolve in a 78°C water bath After that, add the above-mentioned mixed solvent of dimethylformamide and methanol to dilute to the mark, and filter with a 0.45 μm microporous membrane before sample injection for chromatographic analysis.

...

Embodiment 3

[0032] A chromatographic column using octadecyl bonded silica gel as the stationary phase, column length 150mm x inner diameter 4.6mm x packing particle size 5μm, mobile phase is acetonitrile: tetrahydrofuran (containing 0.03% tri-n-octylamine in the total volume of the mobile phase): Water (containing 0.4% citric acid in the total volume of the mobile phase) = 20:10:70, the flow rate is 0.55mL / min, the detection wavelength is 310nm, the column temperature is 40°C, and the injection volume is 20μL. Accurately weigh 20 mg of oxolinic acid sample (batch number 130803) and reference substance respectively, put into a 100 mL volumetric flask, add an appropriate amount of mixed solvent of dimethylformamide and methanol (volume ratio: 2:3), and dissolve in a water bath at 80 °C After that, add the above-mentioned mixed solvent of dimethylformamide and methanol to dilute to the mark, and filter with a 0.22 μm microporous membrane before sample injection for chromatographic analysis.

...

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Abstract

The invention discloses a liquid chromatographic analysis method for determining the content of oxolinic acid and belongs to the field of pharmaceutical and chemical quality inspection technologies. The method comprises the steps: dissolving an oxolinic acid sample to be determined in a mixed solvent prepared from dimethylformamide and methanol which are in the volume ratio of 2: (3-5), so as to obtain a sample solution; determining the content of oxolinic acid in the sample solution by adopting an external standard method, wherein the chromatographic conditions are as follows: a chromatographic column is a C18 column, a moving phase is a mixed solution prepared from acetonitrile, an organic base added organic modifier and an organic acid added water which are in the volume ratio of (10-30): (5-20): (60-90), the flow velocity is 0.3-1.2mL / min, the detection wavelength is 300-350nm, the column temperature is 35-45 DEG C, and the sample size is 5-20 microliters. By adopting the method disclosed by the invention, oxolinic acid can be effectively separated from impurities (A, B and C), so as to accurately determine the content of oxolinic acid; the method has the advantages of simplicity and convenience, reliability, rapidity, high sensitivity and good reproducibility and specificity.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical and chemical quality detection, and in particular relates to a liquid chromatography analysis method for determining the content of oxolinic acid. Background technique [0002] Oxolinic acid, also known as oxycycline oxolinic acid, oxisolinic acid, Oxilinic acid (Oxilinic acid), English abbreviation OA, the second generation product of quinolones, is white with yellowish white columnar crystals or crystalline powder, no Odorless and tasteless, with a melting point of 320°C, almost insoluble in water and ethanol, soluble in formic acid and sodium hydroxide solution, does not absorb moisture, and is relatively stable to heat, humidity and light. It has a strong broad-spectrum, strong antibacterial effect on Gram-negative bacteria and some positive bacteria, and has no cross-resistance with antibiotics, but has no antibacterial effect on fungi and Mycobacterium tuberculosis. It has good antib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 彭要武田文敬徐建义
Owner MASTEAM BIO TECH
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