毛细管气象色谱法测定新药UP0044中有机溶剂的残留量  

Determination of residual organic solvents in a new pharmaceutical-developing(UP0044) by capillary gas chromatography

作　　者：宋文华[1] 孙婷[1] 高敏苓[2] 金星龙[2] 王国峰[3] 

机构地区：[1]天津理工大学环境科学与安全工程学院,天津300191 [2]天津工业大学环境科学与工程研究中心,天津300160 [3]通标标准技术服务有限公司上海分公司生命科学部,上海200233

出　　处：《天津师范大学学报（自然科学版）》2008年第1期28-32,共5页Journal of Tianjin Normal University：Natural Science Edition

基　　金：国家自然科学基金资助项目(30771771);天津市自然科学基金资助项目(06YEJMJC05600)

摘　　要：建立了测定新药UP0044中甲醇、乙醇、二氯甲烷、乙酸乙酯、甲苯、四氢呋喃、乙酸7种有机溶剂含量的方法，以确定它们在药物中的残留量和比例．实验方法采用毛细管气相色谱法，氢火焰离子检测器（FID），以DB-624色谱柱（30m×250pm×1.4μm）对样品进行分离，采取程序升温，载气为氦气，外标法计算含量．结果显示：在各色谱条件下，7种溶剂的线性良好（R^2〉0．99），平均回收率为90％～110％，RSD为1．2％～8．8％，最低检出限0．9×10^-8～1．69×10^-4；所测试的4批样品中除甲醇、乙醇有检出外，其他溶剂均未检出．A method for determining contents of seven kinds of residual organic solvents such as methanol, ethanol, methylene chloride, ethyl aetate, toluene, tetrahydrofuran and acetic acid in a new pharmaceutical-developing （UP0044） was established by capillary gas chromatography. The experimental conditions were DB-624 silica capillary column, FID detector, carrier helium gas and external standard calibration method. The results indicated that the seven residual solvents were separated completely and the linearity were good（R2〉0.99）. Average recovery was 90%-110%, RSD was 1.2%-8.8%. The lowest detection limit was 0. 9×10^-6-1.69× 10^4. Both methanol and ethanol solvents were detected in 4 batches of the UP0044, but other solvents was no done.

关 键 词：UP0044 有机溶剂残留量 气相色谱法 

分 类 号：TQ460.7[化学工程—制药化工]