顶空气相色谱法测定非达霉素原料药中残留溶剂  

Determination of Residual Solvents in Fidaxomicin by Headspace Gas Chromatography

作　　者：邵昉 耿文飞[1] 李晓露[1] 林毅[1] 陆晓菡 刘月[1] 任风芝[1] 张雪霞[1] 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)

机构地区：[1]微生物药物国家工程研究中心河北省工业微生物代谢工程技术研究中心抗体药物研制国家重点实验室,河北石家庄050015 [2]华北制药华胜有限公司,河北石家庄050015

出　　处：《化学与生物工程》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)

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.

关 键 词：顶空气相色谱法 非达霉素 残留溶剂 

分 类 号：O657.3[理学—分析化学]