摘要
目的用毛细管柱气相色谱法建立盐酸伊立替康中残留溶剂(甲醇、无水乙醇、丙酮、三氯甲烷、吡啶)的测定方法。方法采用DB-5(0.53mm×30m,5.00μm)毛细管柱(固定相为5%二苯基-95%二甲基硅氧烷共聚物),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(甲醇r=0.9997,无水乙醇r=0.9997,丙酮r=0.9997,三氯甲烷r=0.9995,吡啶r=0.9998),平均回收率范围为97.3%~101.1%,理论塔板数均>5000,相邻的溶剂峰的分离度均>2,精密度RSD<3%。结论本方法简单、结果准确、重现性好,可用于盐酸伊立替康中甲醇、无水乙醇、丙酮、三氯甲烷、吡啶5种残留溶剂的同时测定。
OBJECTIVE To establish a capillary gas chromatography method for determining the residual solvents. METHODS The capillary was DB-5(0.53 mm×30 m, 5.00 μm). The cartier gas was nitrogen gas and FID was as detector. The injector temperature was set at 200 ℃ and the detector temperature was at 300 ℃. The column temperature program was as follows: initial temperature was at 40 ℃(hold 8 min), with the increase rate of 10 ℃·min^-1 to 120 ℃, and continually increase to 230v at the rate of 35 ℃·min^-1(hold 20 min). The residual solvents were calculated by external standard method. RESULTS A good linearity was obtained in the experimental concentration(r=0.999 5-0.999 8). The recovery was in the range of 97.3%-101.1%. The number of theoretical plates were more than 5 000 and the resolutions among the adjacent peaks were more than 2. The RSDs of precision was all less than 3%. CONCLUSION The methods is simple, sensitive and accurate. It can be used for the detection of five residual solvents in irinotecan hydrochloride.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2009年第18期1426-1428,共3页
Chinese Pharmaceutical Journal
关键词
盐酸伊立替康
气相色谱法
毛细管柱
残留溶剂
irinotecan hydrochloride
gas chromatography
capillary column
residual solvent