毛细管色谱法测定替莫唑胺酯中的有机溶剂残留量  

Determination of residual organic solvents in temozolomide hexyl ester by capillary gas chromatography

作　　者：陈莹[1] 李德馨[1] 王国成[1] 王永峰[1] 

机构地区：[1]天津天士力集团化学制药研究所,天津300402

出　　处：《沈阳药科大学学报》2013年第2期136-138,159,共4页Journal of Shenyang Pharmaceutical University

基　　金：国家"重大新药创制"科技重大专项资助项目(2009ZX09102-058);天津市科技支撑计划重点资助项目(08ZCKFSH03700)

摘　　要：目的建立毛细管气相色谱法测定替莫唑胺酯中的有机溶剂残留量。方法采用INNOWax毛细管气相色谱柱、FID检测器,以乙腈为内标进行测定。结果正己醇、丙酮、乙酸乙酯、异丙醇、正己烷、吡啶的线性范围分别为25～400μg.L-1(r=0.999 6)、25～400μg.L-1(r=0.999 9)、25～400μg.L-1(r=0.999 9)、25～400μg.L-1(r=0.999 7)、1.45～23.2μg.L-1(r=0.999 8)和1～16μg.L-1(r=0.999 3);正己醇、丙酮、乙酸乙酯、异丙醇、正己烷、吡啶的平均回收率分别为99.7%、100.3%、100.2%、100.4%、99.9%和100.3%;RSD分别为1.11%、1.43%、1.47%、1.37%、1.59%和1.47%(n=9)。结论该方法简单、灵敏、准确、重现性好,适用于替莫唑胺酯中的有机溶剂残留量的测定。Objective To develop a gas chromatography method for the determination of residual organic sol- vents in temozolomide hexyl ester. Methods The samples were injected into INNOWax capillary column and analyzed with FID detector using acetonitrile as the internal standard. Results The linear ranges of hexanol, acetone, ethyl acetate, isopropanol, hexane, pyridine were 25- 400 ixg. L - 1 （ r = 0. 999 6 ）, 25- 400 txg. L - 1 （ r = 0. 999 9 ）, 25- 400 ixg. L - 1 （ r = 0. 999 9 ）, 25- 400 ug L -1 （ r = 0. 999 7 ）, 1.45- 23.2 ug. L - 1 （ r = 0. 999 8）, 1 -16 u.L-1 （ r = 0. 999 3 ）, respectively. The recoveries were 99.7%, 100. 3%, 100. 2%, 100. 4% ,99.9%, 100. 3% ; RSD were 1.11%, 1.43%, 1.47%, 1.37%, 1.59%, 1.47% （ n = 9 ）, respec- tively. Conclusions The method is simple, accurate and sensitive with good reproducibility. It can be used for the determination of the residual organic solvents in temozolomide hexyl ester.

关 键 词：替莫唑胺酯 毛细管气相色谱法 有机溶剂残留量 

分 类 号：R917[医药卫生—药物分析学]