Preparation method of high-purity teicoplanin
A high-purity technology for teicoplanin, which is applied in the field of preparation of pharmaceutical raw materials, can solve problems such as poor control of the ratio, no mention of ratio control, cumbersome steps, etc., to achieve reliable quality, controllable content, and process simple effect
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preparation example Construction
[0027] A kind of preparation method of high-purity teicoplanin of the present invention comprises the following steps:
[0028] Step 1) Pretreatment: After the fermented liquid of teicoplanin is adsorbed, concentrated and crystallized by macroporous resin, the crude product of teicoplanin is obtained; the crude product of teicoplanin is dissolved in water or buffered with a pH value of 2-5 Saline solution is dissolved to make an aqueous solution or buffered saline solution of teicoplanin coarse powder; wherein the buffered saline solution is preferably phosphoric acid-diammonium hydrogen phosphate with a pH of 3.5 prepared with 10%~35% (v / v) methanol or ethanol solution.
[0029] Step 2) Chromatography: Add the teicoplanin coarse powder solution to the chromatographic column equipped with nano-polymer microspheres; sequentially use the mixture of polar solvents and water from low to high concentrations for gradient analysis, segmented Collect the analytical solution and perfo...
Embodiment 1
[0034] Take 10 g of the crude product of teicoplanin, with a purity of 81.4%, and dissolve it in 60 mL of deionized water to prepare an aqueous solution of the crude product of teicoplanin. The crude product aqueous solution was loaded on a PSA-30 nano-polymer microsphere chromatographic column with a column size of Ф5.5×50 cm and a loading capacity of 1000 mL. Use 1000mL 25% (v / v) ethanol aqueous solution as the mobile phase for washing, and then use 60% ethanol as the mobile phase to wash until the teicoplanin is resolved, and control the ethanol flow rate to 1500mL / h. Collect analysis solution in sections, according to the HPLC detection result of teicoplanin single component in each section analysis solution, merge analysis solution, make the content of six kinds of single components and A 2 and A 3 The proportion of the group complied with the provisions of the European Pharmacopoeia, and 1570 mL of the analytical solution was obtained. The analysis solution was passed ...
Embodiment 2
[0036] Take 10 g of the crude product of teicoplanin, with a purity of 82.6%, and add it to 50 mL of phosphoric acid-diammonium hydrogen phosphate solution at pH 3.5. The preparation of phosphoric acid-diammonium hydrogen phosphate solution is to dissolve diammonium hydrogen phosphate with a concentration of 5‰ in 30% methanol, and then adjust the pH value to 3.5 with phosphoric acid. After the teicoplanin was dissolved, a buffered saline solution of teicoplanin coarse powder was made, and the solution was loaded on a PS-30 nanopolymer microsphere column (Ф5.5×50cm), with a loading volume of 1000mL. Use 1000mL 30% concentration of methanol as the mobile phase for washing, 60% concentration of methanol as the mobile phase for washing until teicoplanin is completed, the flow rate is 1500mL / h, and the analysis solution is combined according to the HPLC detection results, so that the proportion of each component meets the requirements, and the analysis is obtained. Liquid 1370mL. ...
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