论文部分内容阅读
目的:建立顶空进样气相色谱法检测比卡鲁胺原料药中7种有机残留溶剂二氯甲烷、正己烷、四氢呋喃、乙醇、乙醚、丙酮和乙酸乙酯的方法。方法:色谱柱为Agilent DB-624弹性石英毛细管柱(30.0 m×0.25 mm×1.4μm);进样口温度:200℃;氢火焰离子化检测器(FID)温度:250℃;柱温:程序升温,初始温度35℃,保持13 min,再以100℃/min的速率升至180℃,维持5 min;载气:氮气;流速:1.2 ml·min-1。顶空进样,顶空平衡温度:90℃,顶空平衡时间:30 min;进样体积:1.0 ml;以二甲基亚砜为溶解介质,测定比卡鲁胺中7种溶剂的残留量。结果:各被测溶剂均能良好分离,各溶剂峰面积与浓度均呈良好的线性关系,回收率均较为理想。结论:该法适用于比卡鲁胺原料药中残留溶剂的测定。
OBJECTIVE: To establish a method for the determination of seven organic residual solvents methylene chloride, n-hexane, tetrahydrofuran, ethanol, ethyl ether, acetone and ethyl acetate in headspace sample gas chromatography. Methods: The column was an Agilent DB-624 elastic quartz capillary column (30.0 m × 0.25 mm × 1.4 μm); inlet temperature was 200 ℃; FID temperature was 250 ℃; The initial temperature was maintained at 35 ° C for 13 min and then increased to 180 ° C at a rate of 100 ° C / min for 5 min. The carrier gas was nitrogen and the flow rate was 1.2 ml min-1. Headspace injection, Headspace equilibrium temperature: 90 ℃, Headspace equilibrium time: 30 min; Injection volume: 1.0 ml; Dimethyl sulfoxide as the dissolution medium, Determination of 7 residues in bicalutamide solvent . Results: All the tested solvents could be separated well. The peak area and concentration of each solvent showed a good linear relationship, and the recovery rates were all satisfactory. Conclusion: This method is suitable for the determination of residual solvents in bicalutamide APIs.