摘要
采用顶空气相色谱法,色谱柱为CP8756毛细管柱,顶空平衡温度为70℃,平衡时间为40min,通过程序升温测定非达霉素原料药中4种残留溶剂。结果表明,在3.00~359.48μg·mL^-1范围内,甲醇的浓度与峰面积线性关系良好(R^2=0.9999),平均回收率为98.27%;在2.50~601.03μg·mL^-1范围内,乙醇的浓度与峰面积线性关系良好(R^2=0.9998),平均回收率为98.55%;在2.06~49.44μg·mL^-1范围内,乙腈的浓度与峰面积线性关系良好(R^2=0.9999),平均回收率为99.40%;在1.25~598.60μg·mL-1范围内,乙酸乙酯的浓度与峰面积线性关系良好(R^2=0.9999),平均回收率为98.51%。该方法操作简单、准确度高、重复性好,可用于非达霉素原料药中残留溶剂的质量控制。
We determined four residual solvents in Fidaxomicin by headspace gas chromatography under the conditions as follows:using CP8756 capillary column,the headspace equilibrium temperature of 70℃,the headspace equilibrium time of 40 min,and using programmed temperature rising.The results show that the calibration curves of methanol,ethanol,acetonitrile,ethyl acetate show good linear relationship within the range of 3.00-359.48μg·mL^-1(R^2=0.9999),2.50-601.03μg·mL^-1(R^2=0.9998),2.06-49.44μg·mL^-1(R^2=0.9999),and 1.25-598.60μg·mL^-1(R^2=0.9999),respectively,and the average recoveries are 98.27%,98.55%,99.40%,and 98.51%,respectively.The method is simple,accurate,and repetitive,which can be used for the quality control of the residual solvents in Fidaxomicin.
作者
邵昉
耿文飞
李晓露
林毅
陆晓菡
刘月
任风芝
张雪霞
SHAO Fang;GENG Wenfei;LI Xiaolu;LIN Yi;LU Xiaohan;LIU Yue;REN Fengzhi;ZHANG Xuexia(National Engineering Research Center of Microbial Medicine,Hebei Industry Microbial Metabolic Engineering&Technology Research Center,State Key Laboratory of Antibody Research&Development,Shijiazhuang 050015,China;Huasheng Company of NCPC,Shijiazhuang 050015,China)
出处
《化学与生物工程》
CAS
2019年第8期65-68,共4页
Chemistry & Bioengineering
基金
国家“重大新药创制”科技专项(2019ZX09302006)
关键词
顶空气相色谱法
非达霉素
残留溶剂
headspace gas chromatography
Fidaxomicin
residual solvent
