顶空毛细管气相色谱法测定苦参素注射液中乙醇和丙酮的残留量

目的:建立苦参素注射液中乙醇及丙酮残留量的测定方法。方法:采用气相色谱法,用固定液为6%氰丙基苯基94%二甲基聚硅氧烷(DB-624)的毛细管柱,载气为氮气,氢火焰离子化检测器(FID),进样口温度为200℃,检测器温度为250℃,柱温采用程序升温,初始温度40℃,保持10 min,再以50℃.min-1的升温速率升温至120℃,保持5min。载气流速2.0 mL.min-1,顶空温度为70℃,顶空时间为30 min,顶空进样体积为1 mL。结果:乙醇浓度在9.769～156.3μg.mL-1的范围内,丙酮浓度在16.85～269.6μg.mL-1的范围内具有良好的线性关系。乙醇、丙酮的平均回收率(n=6)分别为93.6%(RSD=1.6%),102.8%(RSD=0.96%)。结论:本方法准确、可靠,灵敏度高,适用于苦参素注射液中乙醇及丙酮残留量的检测。

CGC determination for residual quantity of ethanol and acetone in marine injection with headspace sampling

Objective:To establish a method for the determination of residual quantity of ethanol and acetone in marine injection.Methods:The residual organic solvents were determined by GC with capillary column(DB-624)with FID detector and headspace sampling,which was nitorgen as the carrier gas.The temperature of the injection port was maintaining at 200 ℃ and that of detector at 250 ℃.The oven introduced sequential increasing of temperature programing.The initial column temperature was 40 ℃,maintaining it for 10 min,then raising the temperature to 120 ℃ at a rate of 50 ℃·min-1,and maintaining it at 120 ℃ for 5 min.The flow rate of N2 was 2.0 mL·min-1,headspace oven was set at a temperature of 70 ℃ for 30 min and the injection volume was 1 mL with headspace sampling.Results:The calibration curve showed a good linearity with the range of 9.769-156.3 μg·mL-1 for ethanol and with the range of 16.85-269.6 μg·mL-1for acetone.The average recoveries(n=6)of ethanol and acetone were 93.6%(RSD=1.6%)and 102.8%(RSD=0.96%),respectively.Conclusion:The method is accurate,reliable and sensitive for the determination of the residual quantity of ethanol and acetone in marine injection.