Method for detecting azithromycin capsule related impurities

A technology of azithromycin and detection method, applied in the field of analytical chemistry, can solve the problems such as the increase of the organic phase ratio, the fluctuation of the column pressure and the enlargement

Pending Publication Date: 2020-04-17
HUBEI HONGYUAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection method for azithromycin-related impurities recorded in the European Pharmacopoeia (EP9.0) uses a gradient operation. During the test, the proportion of the organic phase gradually increases, and the column pressure fluctuates gradually when it is mixed with the buffer salt concentration. Drift is easy to occur. Since there are many impuritie

Method used

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  • Method for detecting azithromycin capsule related impurities
  • Method for detecting azithromycin capsule related impurities
  • Method for detecting azithromycin capsule related impurities

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0111] Example 2

[0112] The instruments and chromatographic conditions used are as follows:

[0113] High performance liquid chromatograph: Waters 2695+2998;

[0114] Chromatographic column: Waters XTerra MS C18 column (4.6mm×250mm, 5μm);

[0115] Mobile phase A: methanol-acetonitrile (1:3);

[0116] Mobile phase B: 1.74g / L (0.01mol / L) anhydrous dipotassium hydrogen phosphate solution (use 10% phosphoric acid by volume, or potassium hydroxide solution with 10% mass to volume ratio to adjust the pH to 8.9);

[0117] Perform gradient elution as shown in Table 3 of the mobile phase;

[0118] Table 3 Example 2 Gradient Elution Table

[0119]

[0120] Detection wavelength: 210nm;

[0121] Column temperature: 60℃;

[0122] Flow rate: 1.0ml / min;

[0123] Injection volume: 50μL;

[0124] Diluent: ammonium dihydrogen phosphate solution (weigh 1.73g of ammonium dihydrogen phosphate, dissolve it with water and dilute to 1000ml, adjust the pH value to 10.0±0.05 with ammonia test solution)-methanol-aceto...

Example Embodiment

[0133] Example 3

[0134] The instruments and chromatographic conditions used are as follows:

[0135] High performance liquid chromatograph: Shimadzu LC-16PDA;

[0136] Column: Waters XTerra MS C18 column (4.6mm×250mm, 5μm)

[0137] Mobile phase A: methanol-acetonitrile (1:3);

[0138] Mobile phase B: 1.74g / L (0.01mol / L) anhydrous dipotassium hydrogen phosphate solution (use 10% phosphoric acid by volume, or potassium hydroxide solution with 10% mass to volume ratio to adjust the pH to 8.9);

[0139] The mobile phase was subjected to gradient elution as shown in Table 5;

[0140] Table 5 Example 3 Gradient Elution Table

[0141]

[0142] Detection wavelength: 210nm;

[0143] Column temperature: 60℃;

[0144] Flow rate: 1.0ml / min;

[0145] Injection volume: 50μL;

[0146] Diluent: ammonium dihydrogen phosphate solution (weigh 1.73g of ammonium dihydrogen phosphate, dissolve it with water and dilute to 1000ml, adjust the pH value to 10.0±0.05 with ammonia test solution)-methanol-acetonitrile (7...

Example Embodiment

[0155] Example 4

[0156] The instruments and chromatographic conditions used are as follows:

[0157] High performance liquid chromatograph: Shimadzu LC-16PDA;

[0158] Chromatographic column: Waters XTerra MS C18 column (4.6mm×250mm, 5μm);

[0159] Mobile phase A: methanol-acetonitrile (1:3);

[0160] Mobile phase B: 0.005mol / L anhydrous dipotassium hydrogen phosphate solution (use 10% phosphoric acid by volume, or potassium hydroxide solution with 10% mass to volume ratio to adjust the pH to 8.9);

[0161] The mobile phase was subjected to gradient elution as shown in Table 7;

[0162] Table 7 Example 4 Gradient Elution Table

[0163]

[0164]

[0165] Detection wavelength: 210nm;

[0166] Column temperature: 60℃;

[0167] Flow rate: 1.0ml / min;

[0168] Injection volume: 50μL;

[0169] Diluent: ammonium dihydrogen phosphate solution (weigh 1.73g of ammonium dihydrogen phosphate, add water to dissolve and dilute to 1000ml, adjust the pH to 10.0±0.05 with ammonia test solution)-methanol-aceto...

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Abstract

The invention discloses a method for detecting azithromycin capsule related impurities . A mobile phase for separating the azithromycin related impurities is as follows: a mobile phase A, namely a 0.003 mol/L dipotassium phosphate buffer salt solution; a mobile phase B, namely methanol-acetonitrile (250: 750), and elution detection is carried out by adopting a linear gradient elution method. According to the invention, the azithromycin related impurities can be completely separated, fluctuation of column pressure during detection of the azithromycin capsule related impurities is reduced, the service life of a chromatographic column is prolonged, and impurity judgment errors caused by drifting of peak appearance time are avoided.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to an optimized detection method for azithromycin-related impurities. Background technique [0002] The chemical name of Azithromycin is (2R, 3S, 4R, 5R, 8R, 10R, 11R, 12S, 13S, 14R)-13-[(2,6-dideoxy-3-C-methyl-3-O -methyl-α-L-nucleo-hexapyranosyl)oxy]-2-ethyl-3,4,10-trihydroxy-3,5,6,8,10,12,14-heptamethyl -11-[[3,4,6-trideoxy-3-(dimethylamino)-β-D-xyl-hexapyranosyl]oxy]-1-oxa-6-azacyclopentadecane -15-ketone is a macrolide antibacterial drug. Compared with erythromycin, it is stable to acid, and it is not damaged by gastric acid when taken orally. It has a long half-life, high concentration in tissues and cells at the infection site, and is Gram-negative. The antibacterial effect is expanded, especially the effect on influenza bacillus is strengthened, the antibacterial spectrum is wider, and the antibacterial effect is stronger. [0003] Azithromycin (Azithromyci...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8631
Inventor 王正雄张阳玲朱丽君徐金喜肖伟平何亚娟
Owner HUBEI HONGYUAN PHARMA
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