顶空气相色谱法测定双氢青蒿素磷酸哌喹片中乙醇残留

摘要

目的:建立一种气相色谱法用来测定双氢青蒿素磷酸哌喹片中乙醇残留量.方法:采用顶空自动进样气相色谱在DB-624(6%腈丙基苯基-94%二甲基硅氧烷,30 m×0.53 μm×3.0 μm)毛细管柱中进行测定,以正丙醇为内标物,氮气为载气,柱温:恒温80℃,保持10 min;流速:3.0 ml/min;分流比10∶1;进样口温度:220℃;检测器温度:220℃;顶空瓶平衡温度:80℃,保持30 min.结果:乙醇、正丙醇分离度良好,检测限(limit of detection,LOD)为0.19 μg,定量限(limit of quantitation,LOQ)为0.57 μg.乙醇含量在5.49~109.80 μg范围内,线性关系良好,回归方程为:Y=0.002X+0.003,r=0.999 9.平均回收率为95.63%,RSD=3.32%.结论:该方法可用于双氢青蒿素磷酸哌喹片中乙醇残留量的测定.%Objective: To develop a method to detect the content of residual ethanol solvent in Dihydroartemisinin and Piperaquine Phosphate Tablets by headspace gas chromatography. Methods: DB-624 (6% Cyanopropyl pheny1-94% dimethy polysiloxane, 30 mx0.53 μm×3.0 μm) capillary column and propanol as internal standard were used. The carrier was nitrogen at a flow rate of 3.0 ml/min with the diversion ratio was 10:1. The column temperature was maintained at 80℃ for 10 min. FID detector and inlet temperature was 220℃. The headspace vial was balanced at 80℃ for 30 min. Results: Ethanol and Normal Propyl Alcohol (NPA) had a high resolution, LOD was 0.19 μg, LOQ was 0.57 μg. The linear concentration region of ethanol was 5.49-109.80 μg, r=0.999 9. The relative recovery of ethanol was 95.63% (RSD=3.32%). Conclusion: The method is highly sensitive, accurate and reliable. It can be used for the determination of residual ethanol solvent in Dihydroartemisinin and Piperaquine Phosphate Tablets.