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Three single-component separation methods for Ramoplanin

A separation method and single-component technology, applied in chemical instruments and methods, drug combinations, antibiotics, etc., can solve the problems of expensive equipment, cannot be changed, and small single injection volume, and achieve large injection volume and price. Inexpensive, equivalent separation effect

Inactive Publication Date: 2007-08-29
SHANGHAI INST OF PHARMA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The traditional method of remoplanin (Ramoplanin, A / 16686) purification is described in U.S. Patent (USP4427656) with preparative high-performance liquid chromatography (reversed-phase HPLC, column: μ-BondapackC 18 , diameter 7.8mm × 300mm, mobile phase: ammonium formate and acetonitrile mixed solution) to separate its A1, A2, three single components of A3, the equipment required by this method is expensive, the single injection volume is small, and the preparation liquid phase is due to Need fixed preparation columns, usually these columns are directly produced by the manufacturer, so the size is fixed and cannot be changed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Dissolve the mixture containing three components A1, A2 and A3 of remoplanin with 10% methanol aqueous solution, and in C 18 The upper end of the reverse-phase silica gel column (column height×diameter: 20cm×1cm) was loaded with a sample, and 50% methanol aqueous solution was used as the mobile phase to pass through the column at a flow rate of 0.5ml / min. The effluent containing more than 90% of each component was collected under routine HPLC monitoring. The yield was 83%.

Embodiment 2

[0016] The mixture containing the three components of remoplanin was dissolved in 40% methanol aqueous solution, at C 18 The upper end of the reversed-phase silica gel column (column height×diameter: 20cm×1cm) was loaded with a sample, and 70% aqueous methanol was used as the mobile phase to pass through the column at a flow rate of 2ml / min. The effluent containing more than 90% of each component was collected under routine HPLC monitoring. The yield was 85%.

Embodiment 3

[0018] The mixture containing the three components of remoplanin was dissolved with 20% aqueous methanol solution, and the dissolved matter was vacuum-dried and stored at C 18 The upper end of the reverse-phase silica gel column (column height×diameter: 20cm×1cm) was loaded with a sample, and 60% aqueous methanol was used as the mobile phase to pass through the column at a flow rate of 1ml / min. The effluent containing more than 90% of each component was collected under routine HPLC monitoring. The yield was 82%.

[0019] C used in the above examples 18 The reverse-phase silica gel column packing is Beijing Huideyi Technology Co., Ltd. 20μm-50μm spherical C 18 Reverse-phase silica gel column packing; the remaining reagents are commercially available chromatographically pure.

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PUM

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Abstract

The invention discloses the separating method for the three constituents of Ramoplanin. It includes three constituents of Ramoplanin A1, A2 and A3 that are dissolved by methanol, and taking sampling on the upper end of C18 reverse silica gel column, and using methanol solution as flow passing column to take column chromatography separation. The method has the advantages of low cost and good separation effect.

Description

technical field [0001] The invention relates to a method for separating three single components A1, A2 and A3 of the antibiotic remoplanin. Background technique [0002] The traditional method of remoplanin (Ramoplanin, A / 16686) purification is described in U.S. Patent (USP4427656) with preparative high-performance liquid chromatography (reversed-phase HPLC, column: μ-BondapackC 18 , diameter 7.8mm × 300mm, mobile phase: ammonium formate and acetonitrile mixed solution) to separate its A1, A2, three single components of A3, the equipment required by this method is expensive, the single injection volume is small, and the preparation liquid phase is due to Fixed preparation columns are required, usually these columns are directly produced by the manufacturer, so the size is fixed and cannot be changed. Contents of the invention [0003] The technical problem to be solved by the present invention is to overcome the above-mentioned defects in the prior art, and provide a meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G11/00
Inventor 李继安徐斌
Owner SHANGHAI INST OF PHARMA IND CO LTD