顶空气相色谱法测定双氢青蒿素哌喹片中乙醇残留含量

Determination of residual ethanol solvent in Dihydroartemisinin and Piper aquine Phosphate Tablets by headspace gas chromatography

目的 建立双氢青蒿素哌喹片中乙醇残留检测方法.方法 采用顶空气相色谱法,色谱柱：HP-Innowax（0.32 mm×30 m,0.5 μm）,柱温：程序升温,初始温度50 ℃,保持7 min,以每分钟10 ℃速率升温至150 ℃,保持2 min;进样口温度180 ℃,FID检测器温度250 ℃,正丙醇为内标物,载气为氮气.顶空平衡温度：85 ℃,平衡时间,25 min.结果 乙醇、正丙醇分离度良好,乙醇在0.065 07～1.041 2 mg·mL-1 范围内线性关系良好（r=0.999 9）,平均加样回收率为102.0%,其RSD为2.20%.结论 该方法操作简便快速,灵敏度高,准确度好,可作为双氢青蒿素哌喹片中乙醇残留测定.

Objective To establish a determination method for the residual ethanol solvent in Dihydroartemisinin and Piperaquine Phosphate Tablets. Methods The residual ethanol solvent was determined by headspace gas chromatography on a HP - Innowax column{0. 32 mm ×30 m,0. 5 μm）. The programming temperature of the column was 50 ℃ keeping 7 min,and then to 150 ℃with the increasing rate of 10 ℃ · min-1 keeping 2 min;The injector temperature was 180 ℃ and FID detector temperature was 250 ℃ ;Propanol as internal standard were used and the carrier gas was nitrogen. The headspace vial was balanced at 80 ℃ for 25 min. Results Ethanol and propanol had a high resolution. The linear concentration region of ethanol was 0. 065 07 - 1. 041 2 mg · mL- l （ r = 0. 999 9 ） , The average recoveries of the ethanol was 102. 0% , and the RSD was 2. 20%. Conclusion The method was highly sensitive, accurate and reliable. It can be used for the determination of residual ethanol solvent in Dihydroartemisinin and Piperaquine Phosphate Tablets.