顶空气相色谱法测定奥扎格雷钠中残留溶剂

目的建立奥扎格雷钠中甲醇、乙醇、乙醚、二氯甲烷和三氯甲烷残留量的测定方法。方法采用DB-5毛细管色谱柱(30 m×0.532 mm,1.0μm),载气为氮气,柱温采取程序升温,初始温度40℃,保持4 min,然后以25℃/min的速率升至150℃,保持4 min;顶空进样,进样口温度200℃;氢火焰离子化检测器(FID),检测器温度220℃。结果甲醇、乙醇、乙醚、二氯甲烷和三氯甲烷的线性范围分别为0.26~0.39、0.41~0.62、0.41~0.62、0.071~0.047、4.75~7.12μg/mL,平均回收率(n=9)分别为101.3%、98.2%、95.4%、95.8%、95.4%。结论该方法简便,灵敏度高,重复性好,结果准确,适合奥扎格雷钠中有机溶剂残留量的测定。

Headspace GC determination for residual solutions in sodium ozagrel

Objective To establish a headspace GC method for the determination of residual solution in sodi-um ozagrel. Methods DB-5 column (30 m × 0. 532 mm,1. 0 μm) was adopted,with nitrogen as a carrier gas and FID as a detector. The initial temperature was kept at 40 ℃ for 4 min,and the temperature was raised to 150 ℃ at the rate of 25 ℃/min. The injecting port temperature was 200 ℃,and the detector temperature was 220 ℃. Results The calibration curve of methanol,ether,acetone and carbon dichloride showed a good linearity within the ranges of 0. 26~0. 39,0. 41~0. 62,0. 41 ~0. 62,0. 071 ~0. 047 and 4. 75 ~7. 12 μg/mL. The average recovery rates (n =9) were 101. 3%,98. 2%,95. 4%,95. 8% and 95. 4%,respectively. Conclusion The method is simple,sensitive,reproducible and accurate for the determination of residual solution in sodium ozagrel.