高纯度土霉素碱制备工艺研究 Ⅱ.土霉素新产品中2-乙酰-2-去酰胺土霉素的去除

Study on a new techniquc of the production of high purity oxytetracycline Ⅱ. The isolation of 2-acetyl-2-decarboxamidooxytetracycline from oxytetracycline product

2-乙酰 - 2 -去酰胺土霉素 (ADOTC)是土霉素发酵过程中产生的共生物杂质 ,母环结构与土霉素(OTC)相同 ,所以很难去除。本文提出的沉淀分离方法 ,根据 A酸能与 ADOTC和 OTC形成不同溶解度的络合物的性质 ,使沉淀和溶液分开 ,因而能有效地把 OTC中的 ADOTC分离出来 ,且加入 K4Fe(CN) 6- Zn SO4净化超滤后使 OTC的 HPL C测定纯度由 96 .14%提高到 98.72 % ,ADOTC含量由 1.89%下降到 0 .37%

The isolation of 2 acetyl 2 decarboxamidooxytetracycline (ADOTC) from oxytetracycline (OTC) product by precipitation method was established. ADOTC is one of the major fermentation impurities of OTC and is extremely difficult to be separated. According to the characteristic that acid A and OTC or ADOTC form different complex substances with different solubilities, a method of seperating the ADOTC from OTC by adjusting pH was proposed. The purity of OTC obtained, after K 4Fe(CN) 6 ZnSO 4 was added to remove other impurities, could be improved from 96.14% to 98.72% by HPLC assay, and the content of ADOTC could be decrease from 1.89% to 0.37%.