HPLC analysis method for measuring minocycline and related substances thereof

A technique for minocycline and related substances, which is applied in the field of HPLC analysis for the determination of minocycline and related substances, can solve the problems of low resolution, long analysis time, sensitivity to pH value, etc. tail phenomenon and the effect of improving analysis efficiency

Inactive Publication Date: 2016-02-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Results Although the analytical method successfully realized the analysis of minocycline-related substances, the existing problem was that tetrabutylammonium bisulfate and EDTA used as the mobile phase were very sensitive to the pH value, and it was easy to precipitate and block the chromatographic column. The resolution of the analytical method is not very high
Results Although the analysis method successfully realized the analysis of related substances of minocycline, the existing problem was that N,N-dimethylformamide and tetrahydrofuran used as mobile phases were relatively toxic, which could easily cause some damage to analysts. , and the analysis time is too long, the analysis time is 30min
In addition, although there are many literature reports about the analysis of minocycline, they are all about the analysis of minocycline in complex systems (biological samples), and the analysis of raw material minocycline is of little significance

Method used

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  • HPLC analysis method for measuring minocycline and related substances thereof
  • HPLC analysis method for measuring minocycline and related substances thereof
  • HPLC analysis method for measuring minocycline and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Prepare a 0.1 mg / mL aqueous solution of minocycline and filter it with a 0.45 μm microporous membrane.

[0049] Adopt ZorbaxExtendC18 (Agilent, 250mm * 4.6mm, 5 μm) as chromatographic column, mobile phase is ammonium acetate buffer saline solution (50mmol / L ammonium acetate, 0.1mol / L disodium edetate and triethylamine, three The ratio is 100:10:1)-acetonitrile (ammonium acetate buffer saline solution: acetonitrile volume ratio is 75:25), adjust the pH=9.00 with glacial acetic acid; the detection wavelength is 280nm, the flow rate is 1mL / min, and the injection volume is 20μL , the column temperature is 35°C. Obtain the sample analysis spectrum. As a result, although the baseline separation was achieved and the peak shape was good, the resolution of related substances of minocycline was not high.

Embodiment 2

[0051] Prepare a 0.1 mg / mL aqueous solution of minocycline and filter it with a 0.45 μm microporous membrane.

[0052] ZorbaxExtendC18 (Agilent, 250mm×4.6mm, 5μm) was used as a chromatographic column, and the mobile phase was ammonium acetate buffered saline (250mmol / L ammonium acetate, 0.1mol / L disodium edetate and triethylamine, three The volume ratio is 100:10:1, the same below)-acetonitrile (ammonium acetate buffered saline solution: acetonitrile volume ratio is 75:25), adjust pH=9.00 with glacial acetic acid; detection wavelength is 280nm, flow rate is 1mL / min, The injection volume was 20 μL, and the column temperature was 35°C. Obtain the sample analysis spectrum. As a result, although the baseline separation was achieved and the peak shape was good, the resolution of related substances of minocycline was not high.

Embodiment 3

[0054] Prepare a 0.1 mg / mL aqueous solution of minocycline and filter it with a 0.45 μm microporous membrane.

[0055] Adopt ZorbaxExtendC18 (Agilent, 250mm * 4.6mm, 5 μm) as chromatographic column, ammonium acetate buffer saline (250mmol / L ammonium acetate, 0.1mol / L disodium edetate and triethylamine, the volume ratio of the three 100:10:1)-acetonitrile-methanol (ammonium acetate buffered saline solution: acetonitrile:methanol volume ratio is 75:15:10 volume ratio, the same below), adjust pH=9.00 with glacial acetic acid; detection wavelength is 280nm, flow rate The injection volume was 1 mL / min, the injection volume was 20 μL, and the column temperature was 35 °C. Obtain the sample analysis spectrum. As a result, although the baseline separation was achieved, the peak shape was good, and the resolution of related substances of minocycline basically reached the analysis standard, but the analysis time was too long.

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Abstract

The invention discloses an HPLC analysis method for measuring minocycline and related substances thereof. According to the HPLC analysis method, a chromatographic column Zorbax Extend C18 (250 mm*4.6 mm, 5 micrometers) is adopted, a methanol-acetonitrile-acetate buffer solution serves as a mobile phase, under appropriate ultraviolet detection wavelength and flow velocity, the content of the minocycline is measured through an external standard method, and the content of the related substances of the minocycline is measured through a principal component self-contrasted method. By means of the HPLC analysis method for measuring the minocycline and the related substances thereof, baseline separation of the related substances can be well achieved, the content of the minocycline and related substances thereof can be accurately measured, the method is simple, high in specificity, short in detection time, high in precision and good in repeatability, and a foundation is established for enacting a quality standard of the minocycline.

Description

technical field [0001] The invention relates to an HPLC analysis method for determining minocycline and its related substances. Background technique [0002] Minocycline, chemical name: 4,7-bis(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetra Hydroxy-1,11-dioxo-2-tetracenecarboxamide, also known as minocycline, is a broad-spectrum antibacterial tetracycline antibiotic, which has a wider antibacterial spectrum and antibacterial properties than similar tetracyclines. Activity and high fat solubility, in many tissues and body fluids where antibiotics are difficult to penetrate, can reach a high concentration, and can maintain a long time, and the oral effect is good, therefore, minocycline is the current clinical One of the most widely used tetracycline antibiotics. The chemical structural formula is: [0003] [0004] At present, although there are some literature reports about the analysis method of minocycline-related substances, there are some defects, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/74
CPCG01N30/60G01N30/74
Inventor 任钟旗李蕾蕾周智勇张帆孔德隆
Owner BEIJING UNIV OF CHEM TECH
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