顶空气相色谱法检测多烯紫杉醇原料药中有机溶剂残留量  

Determination of Residue Levels of Organic Solvents in Docetaxel by Head Space GC

作　　者：战寒秋[1] 刘冬[2] 赵敬华[3] 吕昭云[2] 兰培[2] 李桦[2] 王茜[2] 史录文[4] 

机构地区：[1]北京地坛医院,北京市100015 [2]中国医学科学院药物研究所,北京市100050 [3]北京市医疗保险事务管理中心,北京市100050 [4]北京大学药学院,北京市100091

出　　处：《中国药房》2009年第25期1982-1984,共3页China Pharmacy

摘　　要：目的:建立检测多烯紫杉醇原料药中甲醇、二氯甲烷等8种有机溶剂残留量的方法。方法:采用气-质联用方法鉴定在初步试验中发现的2种未知溶剂峰,顶空气相色谱法分析检测8种有机溶剂,色谱条件:色谱柱为HP-5,载气为氮气,检测器为氢火焰离子化检测器,进样口温度为180℃,检测器温度为250℃,柱温采用程序升温,流速为1.7mL·min-1,分流比为1∶10,进样方式为顶空进样,进样体积为1.0mL。结果:确定了2种未知有机溶剂为3-甲基戊烷和甲基环戊烷;8种溶剂在各自对应的浓度范围内线性关系良好(r>0.9973),回收率>91.3%(RSD<3.8%,n=5)。结论:所建方法灵敏、准确、可靠,适用于同时分析检测多烯紫杉醇中的8种有机溶剂。OBJECTIVE： To established a method for determination of residue levels of 8 organic solvents including methanol and dichlormethane in docetaxel crude drug. METHODS： GCMS was employed to identify the peaks of two un-known residual solvents in docetaxel, and head space GC was employed to determined 8 organic solvents. The chromatographic condition was as follows： the chromatographic column was HP-5; the carrier gas was nitrogen gas; the detector was flame ionization detector which was kept at 250℃; the injector temperature was 180℃. The column temperature was programmed raised; the flow rate was 1.7 mL·min^-1; the split ratio was 1 ： 10; the sample was injected by head space injection with an injection volume of 1.0 mL. RESULTS： The unknown residual solvents in docetaxel were determined as 3-methylpentane and methylcyclopentane. The 8 solvents showed good linear relationship within a certain concentration range （r 〉0.9973） and their average recovery rates were all above 91.3% （RSD〈3.8%, n = 5）. CONCLUSION： This method is sensitive, accurate and reliable and it can be applied for the determination of residue level of organic solvents in docetaxel.

关 键 词：多烯紫杉醇 顶空气相色谱法 有机溶剂 残留量 

分 类 号：R927.2[医药卫生—药学] R979.1