摘要
目的:用毛细管柱气相色谱法建立苯磺阿曲库铵中残留溶剂(乙醚、丙酮、甲醇、二氯甲烷、乙腈、甲苯)的测定方法。方法:采用DM-Wax(30 m×0.53 mm,1.00μm)毛细管柱(固定相为键合交联聚乙二醇),以氮气为载气,FID检测器,采用程序升温,分流直接进样,外标法计算残留溶剂的含量。结果:在考察的浓度范围内呈现良好的线性关系(乙醚r=0.9997,丙酮r=0.9997,甲醇r=0.9996,二氯甲烷r=0.9996,乙腈r=0.9991,甲苯r=0.9997),平均回收率范围为97.4%～99.7%,理论塔板数均>7000,相邻的峰之间的分离度均>2,精密度、重复性RSD均<3%。结论:本方-法简单、结果准确、重现性好,可用于苯磺阿曲库铵中乙醚、丙酮、甲醇、二氯甲烷、乙腈、甲苯6种残留溶剂的同时测定。
Objective：To establish a method for determining the residual of solvents by capillary gas chromatography.Method：The capillary was DM-Wax（30m×0.53 mm,1.00μm）.The carrier gas was nitrogen gas and FID was as detector.The injector temperature was set at 150℃and the detector temperature was 200 ℃.The column temperature program was initial temperature 60℃（hold 5 min）,with the increase rate of 40℃·min^-1to 120℃（hold 7min）.The residual solvents were calculated by external standard method.Results：A good linearity was obtained in the experimental concentration（r=0.9991～0.9997）.The recovery was in the range of 97.4%～99.7%.The number of theoretical plates were more than 7000 and the resolutions between the adjacent peaks were more than 2.The RSDs of precision and accuracy was all less than 3%.Conclusion：The methods is simple,sensitive and accurate.It can be used for detection of six residual solvents in atracurium besilate.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2008年第1期56-59,共4页
Chinese Journal of New Drugs
关键词
气相色谱法
苯磺阿曲库铵
毛细管柱
残留溶剂
gas chromatography
atracurium besilate
capillary column
residual solvent
