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Fidaxomicin impurities and preparation method thereof

A technology for fidaxomicin and impurities, which is applied in the field of pharmaceutical analysis, can solve the problems of few studies on degrading impurities, and achieve the effect of improving quality controllability and quality improvement

Inactive Publication Date: 2019-08-30
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, little research has been done on degrading impurities

Method used

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  • Fidaxomicin impurities and preparation method thereof
  • Fidaxomicin impurities and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The detection of embodiment 1 impurity F

[0036] Instrument: Agilent 1260 HPLC

[0037] Chromatographic conditions: Chromatographic column: Agilent Poroshell 120EC-C18 (100*4.6mm, 2.7μm); mobile phase: 0.05M potassium dihydrogen phosphate solution-acetonitrile (50:50), isocratic elution; column temperature: 15°C; Flow rate: 0.5ml / min; detection wavelength: 230nm.

[0038] Dissolve the fidaxomicin sample in methanol solution to prepare a sample solution with a concentration of 0.5 mg / ml; inject the sample solution into a liquid chromatograph. Detected by HPLC, the impurity peak at relative retention time (RRT) 1.33 is impurity F, see attached figure 1 .

Embodiment 2

[0039] The preparation of embodiment 2 impurity F

[0040] Instrument: Gilson GX-281 preparative chromatography system, rotary evaporator: Shensheng rotary evaporator LABOROTA4001

[0041] Chromatographic conditions:

[0042] Chromatographic column: Agilent ZORBAX RX-C18, with octadecylsilane bonded silica gel as filler, the column length of this chromatographic column is 250 mm, and the inner diameter is 21.2 mm.

[0043] Detection wavelength: 230nm; flow rate: 15ml / min, injection volume: 8ml

[0044] Mobile phase: acetonitrile-water-acetic acid (52:48:1)

[0045] Mix 40ml of acetonitrile, 60ml of water and 1ml of acetic acid to prepare a mixed solution of acetonitrile-water-acetic acid, dissolve the pretreated fidaxomicin sample at 60°C in the mixed solution of acetonitrile-water-acetic acid to make a concentration of 20mg / ml solution. According to the above-mentioned chromatographic conditions, the fractions for 28-32 minutes were collected, and the impurity target frac...

Embodiment 3

[0047] The preparation of embodiment 3 impurity F

[0048] Apparatus and reagents are the same as in Example 2.

[0049] Detection wavelength: 230nm; flow rate: 10ml / min, injection volume: 2ml

[0050] Mobile phase: acetonitrile-water-acetic acid (52:48:1)

[0051] Mix 20ml of acetonitrile, 40ml of water and 0.5ml of acetic acid to prepare a mixed solution of acetonitrile-water-acetic acid, and dissolve the pretreated fidaxomicin sample at 60°C in the mixed solution of acetonitrile-water-acetic acid to make a concentration of 5mg / ml The solution. The fractions collected for 43-47 minutes were collected according to the above-mentioned chromatographic conditions, and the impurity target fraction was confirmed by the fidaxomicin liquid chromatography analysis method. Samples were injected continuously, the target components were collected and combined, concentrated and dried by rotary evaporation to obtain a white solid.

[0052] The obtained white solid was detected by HPLC...

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Abstract

The invention provides fidaxomicin new impurities and a preparation method thereof. The impurities can be applied to quality control of fidaxomicin raw materials and / or preparations, and is used for impurity contrast positioning, quality determination or quantity determination in the fidaxomicin raw materials and / or preparations, and improvement of the quality of the fidaxomicin raw materials and / or preparations is facilitated.

Description

technical field [0001] The invention belongs to the technical field of medical analysis, and in particular relates to a fidaxomicin impurity F and its preparation method and application. Background technique [0002] Fidaxomicin (trade name Dificid) is the first of the new oral narrow-spectrum macrocyclic antibiotics developed by Optimer. Actinoplans deccanensis or Dactylosporangium aurantiacum fermentation product. Molecular weight 1058.04, molecular formula C 52 h 74 C 12 o 18 , the structural formula is shown in the following formula (A). [0003] [0004] Fidaxomycin has a novel mechanism of action, mainly through the inhibition of bacterial RNA polymerase to produce a rapid anti-refractory Clostridium infection (CDI) effect. [0005] The MIC50 and MIC90 of fidaxomicin against Clostridium difficile were significantly lower than those of vancomycin or metronidazole, and the treatment reduced the recurrence rate and overall cure rate of Clostridium difficile infec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 李鑫健雍春胡帅帅
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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