摘要
目的 建立顶空气相色谱法测定卡巴他赛中甲醇、乙醇、丙酮、二氯甲烷和正己烷共5种有机溶剂的残留量。方法采用顶空气相色谱法,氢火焰离子化检测器;载气为氮气,流速为2.0 m L·min-1;色谱柱为DB-624毛细管柱（30 m×530μm,3μm）;采用柱温50℃保持7 min,以50℃·min-1的速率升温至220℃,保持3 min;进样口温度为200℃,检测器温度为250℃;分流进样,分流比为5∶1;顶空平衡温度为100℃,顶空平衡时间为20 min;顶空定量环体积为1 m L。以外标法用峰面积计算残留溶剂的含量。结果 甲醇、乙醇、丙酮、二氯甲烷和正己烷的线性关系良好（r=0.997 8～0.999 5）,平均回收率为94.0%～99.1%,检测限分别为0.67、0.64、0.23、0.94和0.03 mg·L-1。结论 本方法可用于卡巴他赛中残留溶剂的检查。
Objective To establish a method for determination of five kinds of residual solvents in cabazitaxel by headspace gas chromatography. Methods The residual solvents were separated on DB-624 （30 m × 530 μm,3 μm）capillary chromatography column equipped with FID detector. The carries gas was nitrogen with the flow rate of 2. 0 mL. min - 1. The initial temperature of column was set at 50 ℃ and maintained for 7 min, and then followed by raising the temperature to 220 ℃ with a rate of 50 ℃. min -1 and maintaining for 3 min. The inlet temperature was 200 ℃ and the FID detector temperature was 250 ℃. Split ratio was 5： 1. The temperature of the headspace oven was heated to 100 ℃ and lasted for 20 rain. The injection volume was 1.0 mL. The content of residual solvents was calculated by using external standard method. Results There was a good linear relationship in the experimental concentrations of five residual solvents （ r =0. 997 8 -0. 999 5）. The average recovery ranged from 94. 0% to 99. 1%. The limit of detection was 0. 67,0. 64,0. 23,0. 94, and 0. 03 mg. L - 1 respectively. Conclusions The method can be used for detection of residual solvents in cabazitaxel.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2016年第9期718-722,共5页
Journal of Shenyang Pharmaceutical University
关键词
卡巴他赛
顶空气相色谱法
残留溶剂
cabazitaxel
headspace gas chromatography
residual solvent
