顶空气相色谱法测定双氢青蒿素哌喹片中乙醇残留含量

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,0.5μm),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2min;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,25min。结果乙醇、正丙醇分离度良好,乙醇在0.065 07¹.041 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。

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

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.