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A method for separating and detecting azithromycin and its impurities

A technology for azithromycin and impurities, which is applied in the field of separation and detection of azithromycin and its impurities, which can solve the problems of high chromatographic column loss, low detection sensitivity, and high column temperature, and achieve high sensitivity, simple and convenient operation, and low column temperature.

Active Publication Date: 2016-03-02
SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is to overcome the defects of low detection sensitivity of the existing method for separating and detecting azithromycin and its impurities, high column temperature of the adopted chromatographic column, and large loss to the chromatographic column, and a separation method is provided. Method for detecting azithromycin and its impurities

Method used

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  • A method for separating and detecting azithromycin and its impurities
  • A method for separating and detecting azithromycin and its impurities
  • A method for separating and detecting azithromycin and its impurities

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Embodiment 1

[0038] Column: XBridge TM C18 column (250mm×4.6mm, 5 μm); column temperature: 40°C; preparation of mobile phase A: aqueous solution of formic acid with a volume fraction of 0.3%, adjust its pH value to 8.20 with ammonia water, mobile phase B is acetonitrile:methanol=3 :1, linear gradient elution: 0min:70%A+30%B→30min:70%A+30%B→50min:45%A+55%B→53min:45%A+55%B→65min: 30%A+70%B; flow rate: 1.0mL / min; detection wavelength: 210nm; injection volume: 10μL. The fractions after liquid chromatography were detected by ultraviolet light and entered into mass spectrometer for detection in a 3:1 split.

[0039] Take 10 mg of azithromycin raw material drug (batch number 20120423), dissolve it in acetonitrile, prepare a solution with a concentration of 1 mg / ml, and inject a sample volume of 10 μL. According to the separation and detection of liquid chromatography-mass spectrometry, a total of 10 related impurities (such as figure 1 shown). As can be seen from the figure, the method of the pr...

Embodiment 2

[0041] Column: XBridge TM C18 column (250mm * 4.6mm, 5 μ m); Column temperature: 40 ℃; Mobile phase A is the solution that forms when the pH value of the formic acid aqueous solution of 0.3% is adjusted to 8.20 with ammoniacal liquor, and mobile phase B is acetonitrile:methanol= 3:1, linear gradient elution: 0min:70%A+30%B→30min:70%A+30%B→50min:45%A+55%B→53min:45%A+55%B→65min : 30%A+70%B; flow rate: 1.0mL / min; detection wavelength: 210nm; injection volume: 10μL. The fractions after liquid chromatography were detected by ultraviolet light and entered into mass spectrometer for detection in a 3:1 split.

[0042] Dissolve azithromycin and 11 kinds of impurity reference substances (impurities A, B, E, F, G, H, I, J, L, M, N) into acetonitrile and ultrasonically dissolve, prepare a solution with a concentration of 1mg / ml, and inject The volume is 10 μ L, according to liquid chromatography-mass spectrometry separation and detection, azithromycin and various impurities have achieve...

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Abstract

The invention discloses a method of separating and detecting azithromycin and impurities of the azithromycin. The method includes following steps of: dissolving an azithromycin sample into acetonitrile to form a sample solution, and separating and detecting the azithromycin and the impurities by a liquid chromatography-mass spectrometry method. Conditions of the liquid chromatography-mass spectrometry method are that: a chromatographic column adopts an octadecylsilane-bonded silica gel chromatographic column; a mobile phase A is prepared by preparing an aqueous formic acid solution having a volume percentage of 0.3% and adjusting the pH to 8.20 with aqueous ammonia; a mobile phase B is a mixed solution of acetonitrile and methanol in a volume ratio of 3:1; the mobile phase A and the mobile phase B are adopted to perform linear gradient elution; the flow rate is 1.0 mL / min; the detection wave length of an ultraviolet detector is 210-215 nm; and one fifth to one third of a flow part after the ultraviolet detector enters a mass spectrometer to be detected. The method provided by the invention is high in detection sensitivity. The column temperature of the adopted chromatographic column is low. Operation is simple and convenient.

Description

technical field [0001] The invention relates to the field of drug detection, in particular to a method for separating and detecting azithromycin and its impurities. Background technique [0002] Azithromycin (Azithromycin) is a 15-membered azamacrolide compound synthesized by Beckmann rearrangement, reduction, and N-methylation reactions after 9-ketooximation on erythromycin A. Developed by Pliva in the late 1970s, it was later transferred to Pfizer and sold globally under the trade name of Zithromax. The antibacterial mechanism of azithromycin is similar to that of erythromycin. It binds to the ribosomal 50S subunit in bacterial cells, hinders the bacterial transpeptide process, and inhibits the synthesis of RNA-dependent proteins to achieve antibacterial effects. Compared with erythromycin, azithromycin has a wider antibacterial spectrum, can inhibit a variety of gram-positive cocci, mycoplasma, chlamydia and Legionella pneumophila, especially for some important gram-nega...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/60
Inventor 李悦许卓妮沈舜义
Owner SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
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