论文部分内容阅读
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 headspace gas chromatographic method for the determination of the residues of 5 organic solvents in methanol, ethanol, acetone, methylene chloride and n-hexane in cabazitaxel. The method was characterized by headspace gas chromatography and flame ionization detector. The carrier gas was nitrogen and the flow rate was 2.0 m L · min-1. The column was DB-624 capillary column (30 μm × 530 μm, 3 μm) 50 ℃ for 7 min, at a rate of 50 ℃ · min-1 temperature was raised to 220 ℃ for 3 min; inlet temperature was 200 ℃, detector temperature was 250 ℃; split injection, split ratio of 5: 1; Headspace equilibrium temperature of 100 ° C, headspace balance time of 20 min; headspace quantitative ring volume of 1 m L. External standard method to calculate the peak area of residual solvent content. Results The linear relationship between methanol, ethanol, acetone, methylene chloride and n-hexane was good (r = 0.997 8 ~ 0.999 5), and the average recovery was 94.0% ~ 99.1%. The detection limits were 0.67,0.64,0.23,0.94 and 0.03 mg · L-1. Conclusion This method can be used for the determination of residual solvents in cabazitaxel.