气相色谱法同时测定盐酸坦洛新原料药中4种有机溶剂残留量

摘要

Objective To establish a method of determining 4 kinds of residual organic solvents(methanol,ethanol,acetonitrile, dichloromethane) in tamsulosin hydrochloride raw medicine. Methods Capillary gas chromatography was adopted,the column was DB-FFAP capillary gas chromatography column(30 m × 0. 53 mm,3. 0 μm),the carrier gas was nitrogen with hydrogen flame ionization de-tector. The temperature was programmed to be 40 ℃ for 6 min,and then programmed to be 200 ℃ at 30 ℃ /min to maintain for 5 min. The inlet temperature was 200 ℃,the detector temperature was 250 ℃,and the split ratio was 20:1. Results The 4 kinds of organic solvents were separated completely,The mass concentrations of methanol,ethanol,acetonitrile and dichloromethane were linear in the range of 13. 50 -270. 00 ,11. 56 -231. 20 ,9. 57 -191. 32 ,1. 36 -27. 20 μg / mL . The results of recovery test were good . Conclusion The sensitivity and accuracy of the method can meet the requirement of organic solvent residue. It is suitable for the de-termination of residual organic solvents in tamsulosin hydrochloride raw medicine.%目的 建立盐酸坦洛新原料药中有机溶剂(甲醇、乙醇、乙腈、二氯甲烷)残留量的测定方法.方法 采用毛细管气相色谱法.色谱柱为DB-FFAP毛细管气相色谱柱(30 m×0.53 mm,3.0μm),载气为氮气,氢火焰离子化检测器;程序升温,40℃保持6 min,后以30℃/min的速率升温至200℃,保持5 min;进样口温度200℃,检测器温度250℃,分流比为20:1.结果 4种有机溶剂完全分离,甲醇、乙醇、乙腈、二氯甲烷质量浓度分别在13.50~270.00,11.56~231.20,9.57~191.32,1.36~27.20μg/mL范围内与峰面积比线性关系良好,加样回收试验结果理想.结论 所建立的检测方法灵敏度和准确度均达到有机溶剂残留量的检测要求,适用于坦洛新原料药中有机溶剂残留量的检测.