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作 者:李国亮[1] 苏旭霞[2] 王鲁燕[1] 戈梅[2] 陈代杰[2]
机构地区:[1]中国药科大学生物制药学院,南京210009 [2]上海来益生物药物研究开发中心,上海201203
出 处:《中国抗生素杂志》2002年第11期661-663,共3页Chinese Journal of Antibiotics
摘 要:建立了一种采用高效液相测定发酵液中小组分环孢菌素D含量的方法。发酵液经甲醇提取 ,浓缩至干 ,乙醚转移 ,蒸干 ,甲醇定容 ,正已烷脱脂后进样。色谱条件为YWG C1 8柱 (5μm ,4 6mm× 2 50mm) ;乙腈—水 (78∶2 2 ,v/v)为流动相 ;流速 1 0ml/min ;检测波长 2 2 0nm ,柱温 70℃。该方法的精密度、线性关系和回收率均良好 ,且操作方便 ,比较成功地解决了在杂质较多和含量较低情况下环孢菌素D的测定。A HPLC method was establishd to determine the minor component of cyclosporin D in fermentation broth. Samples were extracted by methanol and concentrated to dryness. And then, the concentrated samples were dissolved in ether. After removing the insoluable mass and evaporating the ether, the samples were reextracted by methanol, removing the endogenous interference substance in samples with n hexane, the samples were analyzed by HPLC. The chromatographic conditions were as follows: YWG C 18 column (5μm, 4 6mm×250mm) and VWD UV detector at 220nm, temperature 70℃. The mobile phase was acetonitrile water (78∶22, v/v). The flow rate was 1.0ml/min. The precision, linear relationship and recovery rate of this method were good. This method was convenient and rapid to determine the cyclosporin D in fermentation broth.
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