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Method for separating and purifying thiopeptide antibiotic nocathiacin I through reversed-phase column

A nocafloxacin and purification method technology, which is applied in the field of separation, purification and purification of antibiotics, can solve the problems of complex structure of nocafloxacin I, low purity of nocafloxacin I, limited purification ability, etc., and achieve high product quality, Small environmental pollution and good repeatability

Inactive Publication Date: 2013-08-07
CHINA PHARM UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Nocafloxacin I has a complex structure and is mainly obtained through microbial fermentation and extraction. The purity of nocafloxacin I obtained by this method is low and cannot meet the needs of preclinical and clinical research. Currently, it is mainly obtained through normal phase silica gel column chromatography. Purify nocafloxacin I, but this method has limited purification capacity, low recovery rate, heavy workload, and high cost (see: Chinese invention patent with patent number 99898680.0)

Method used

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  • Method for separating and purifying thiopeptide antibiotic nocathiacin I through reversed-phase column

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Weigh a certain amount of reversed-phase silica gel with a particle size of 40-75 μm, and after methanol treatment, fill and balance. Crude nocafloxacin I was dissolved in DMSO at concentrations of 25 and 150 mg / mL, respectively. Add the sample solution containing the crude product of nocafloxacin I (the mass ratio of nocafloxacin to silica gel is 1:2000--1:12000) to the top of the reversed-phase silica gel column respectively, open the valve, and wait until the sample liquid level is close to At the edge of the column surface, add about 5 times the column volume of 35% acetonitrile to elute, and then use 38% acetonitrile to elute about 4 times the column volume. Collect 38% of the acetonitrile eluate in a volume of 5-8 mL per tube, monitor in real time by thin-layer chromatography, combine all components containing nocafloxacin I, remove acetonitrile and extract with 2 times the volume of ethyl acetate, extract The liquid was evaporated to dryness to obtain high-purit...

Embodiment 2

[0031] Weigh a certain amount of reversed-phase silica gel with a particle size of 20-45 μm, and after methanol treatment, fill and balance. Crude nocafloxacin I was dissolved in DMSO at a concentration of 25 mg / mL. Add the sample solution containing nocafloxacin I crude product (the mass ratio of nocafloxacin to silica gel is 1:2000--1:12000) dropwise to the top of the reversed-phase silica gel column, open the valve, wait until the sample liquid level is close to the column At the edge of the material surface, add about 3 times the column volume of 45% acetonitrile to elute, and then use 50% acetonitrile to elute about 3 times the column volume. Collect 50% of the acetonitrile eluate with a volume of 5-8 mL per tube, monitor in real time by thin-layer chromatography, combine all components containing nocafloxacin I, remove acetonitrile and extract with 2 times the volume of ethyl acetate, extract The liquid was evaporated to dryness to obtain high-purity nocafloxacin I. Th...

Embodiment 3

[0033] Weigh a certain amount of reversed-phase silica gel with a particle size of 70-200 μm, after methanol treatment, fill and balance. Crude nocafloxacin I was dissolved in DMSO at a concentration of 25 mg / mL. Add the sample solution containing nocafloxacin I crude product (the mass ratio of nocafloxacin to silica gel is 1:12000--1:2000) dropwise to the top of the reversed-phase silica gel column, open the valve, wait until the sample liquid level is close to the column At the edge of the material surface, add about 5 times the column volume of 30% acetonitrile to elute, and then use 35% acetonitrile to elute about 3 times the column volume. Collect 35% of the acetonitrile eluate in a volume of 5-8 mL per tube, monitor in real time by thin-layer chromatography, combine all components containing nocafloxacin I, remove acetonitrile and extract with 2 times the volume of ethyl acetate, extract The liquid was evaporated to dryness to obtain high-purity nocafloxacin I. The pur...

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Abstract

The invention relates to a method for purifying thiopeptide antibiotic nocathiacin I through reversed-phase column chromatography. The method comprises the following steps of: dissolving a nocathiacin I crude product in dimethylsulfoxide (DMSO), then carrying out a reversed-phase column chromatography so as to purify the nocathiacin I through gradient elution, collecting eluent containing only nocathiacin I, evaporating out an organic solvent under reduced pressure, extracting an aqueous phase by ethyl acetate or chloroform, separating and evaporating an extracting agent to dryness, thus obtaining the product. The method is simple to operate; the high-purity nocathiacin I can be obtained through one-step column chromatography; and the purity of the nocathiacin I is more than 98.0%, the yield of the nocathiacin I reaches up to 85.0%, and solvents adopted in multiple steps can be recycled.

Description

technical field [0001] The invention relates to a method for separating and purifying the thiopeptide antibiotic nocafloxacin I by a reversed-phase column, and belongs to the technical field of antibiotic separation, purification and purification. Background technique [0002] Since Fleming discovered penicillin in 1928 and Waxman discovered streptomycin in 1942, antibiotics have made outstanding contributions to human health. When people use antibiotics to treat diseases, they also exercise the drug resistance of bacteria, so with the abuse of antibiotics and the rapid evolution of pathogenic bacteria, more and more drug-resistant strains have appeared clinically, especially for multi- Strains resistant to all kinds of antibiotics, such as methicillin-resistant Staphylococcus aureus (MRSA) and penicillin-resistant Streptococcus pneumoniae (PRSP), people are often helpless in the face of the rapid infection rate of such strains. With the gradual increase of Gram-positive ba...

Claims

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Application Information

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IPC IPC(8): C07K5/078C07K1/16B01D15/32
Inventor 陈依军朱天翼
Owner CHINA PHARM UNIV
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