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Separation, preparation and purification method of gamithromycin related substance

A technology of gamycin and related substances, which is applied in the field of preparation and purification, and the separation of gamitomycin-related substances, and can solve problems such as inability to identify, incapable of gamitycin quality control, and lack of gamitomycin-related substances. , to achieve the effect of simple process and high yield

Pending Publication Date: 2020-01-07
LUOYANG HUIZHONG ANIMAL MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the defects in the prior art that there are no related substances of gamithromycin with a definite structure, and the related substances of gamithromycin cannot be identified and the quality of gamithromycin can not be controlled. The present invention provides a related Substance, its preparation method, and separation and analysis method

Method used

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  • Separation, preparation and purification method of gamithromycin related substance
  • Separation, preparation and purification method of gamithromycin related substance
  • Separation, preparation and purification method of gamithromycin related substance

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1. The detection method of Gamithromycin related substances

[0046] Dissolve 5 mg of the synthetic crude product of gamithromycin in 1 ml of acetonitrile, and the injection volume is 20 μl. The chromatographic parameters are: the mobile phase is a mixed system of 0.05% trifluoroacetic acid aqueous solution and acetonitrile, the flow rate is 20ml / min, the column temperature is 40°C, and the preparative chromatographic column used is Phenomenex Kintex (5 μm, 150×30mm). The gradient changes are shown in Table 1:

[0047] Table 1 The change of mobile phase with time

[0048] time (min) B% (acetonitrile) 0 10 10 25 10.1 75 12 85 12.1 15

[0049] The HPLC fraction passes through the UV detector and then splits into the MS detector. The total ion flow of the mass spectrometer is as follows: figure 1 Shown, each impurity is shown in table 2 below, from figure 1 As can be seen in the above HPLC method can be used to detect...

Embodiment 2

[0054] Embodiment 2. Related substances produced by different degradation reactions of gamithromycin

[0055] 2.1 Research on acid degradation products

[0056] Take about 100 mg of gamimycin (batch number: 20140901), accurately weigh it, place it in a 10 mL measuring bottle, add 1 mL of 0.3 mol / L hydrochloric acid solution, let it stand at room temperature for 10 minutes, add 0.3 mol / L sodium hydroxide solution to adjust to neutral properties, add diluent to dissolve to volume. image 3 It is the HPLC spectrum of the degradation product of gamimycin acid.

[0057] 2.2 Research on Alkaline Degradation Products

[0058] Take about 100 mg of gamimycin (batch number: 20140901), weigh it accurately, put it in a 10 mL measuring bottle, add 1 mL of 1 mol / L sodium hydroxide solution, heat it in a water bath at 100 ° C for 11 h, add 1 mol / L hydrochloric acid to adjust to Neutral, add diluent to dissolve to volume. Figure 4 It is the HPLC spectrum of the degradation product of gar...

Embodiment 3

[0068] The preparation of embodiment 3 Gamithromycin related substances

[0069] Gamithromycin 10g, add 100ml of chloroform, add 2.0-5.0ml of hydrogen peroxide under stirring, heat up to 62-65°C and reflux, react for 1h, cool down to 0-5°C in an ice-water bath, add saturated sodium bisulfite solution at low temperature Quench, separate layers, and evaporate the organic phase to dryness under reduced pressure (0.1 atmosphere pressure≥vacuum degree≥0.093 atmosphere pressure, temperature 30°C) to obtain 8.8 g of crude carmimycin-related substances.

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Abstract

The invention discloses a gamithromycin related substance. The gamithromycin related substance is a compound or salt thereof having a structural formula as shown in a formula (I). The gamithromycin related substance can provide guarantee for monitoring the quality of gamithromycin. The invention further discloses a preparation, analysis and separation method of the gamithromycin related substance.The preparation method disclosed by the invention is simple in technology, and can be in large-scale application in the industry.

Description

technical field [0001] The invention belongs to the technical field of chemical medicines, and in particular relates to a method for separating, preparing and purifying related substances of gamimycin. Background technique [0002] Gamithromycin is a semi-synthetic macrolide antibiotic. Gamithromycin is a fifteen-membered macrocyclic endogenous compound obtained by isomerization, rearrangement reduction and propylation of erythromycin A oxime (type E). Ester antibiotics, compared with azithromycin and telamycin, which are semi-synthetic macrolides with 15-membered rings, gamithromycin has undergone an isomerization step in the early synthesis, resulting in the position of N on the ring after ring expansion different. Gamithromycin contains two polar groups in its structure, and belongs to diamine macrolide antibiotics, which are quite different from azalide and ketolide antibiotics. [0003] Gamithromycin was launched in the European Union in 2007 for the treatment and pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/06C07H1/00G01N30/89
CPCC07H17/00C07H1/06C07H1/00G01N30/89
Inventor 张许科侯林
Owner LUOYANG HUIZHONG ANIMAL MEDICINE
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