期刊文献+

顶空气相色谱法同时测定法匹拉韦原料药中5种有机溶剂的残留量 被引量:8

Simultaneous Determination of 5 Organic Solvents in Favipiravir by Headspace GC
下载PDF
导出
摘要 目的:建立同时测定法匹拉韦原料药中乙醇、丙酮、乙酸乙酯、N,N-二异丙基乙胺、甲苯5种有机溶剂残留量的方法。方法:采用顶空气相色谱法。色谱柱为DB-624毛细管柱,程序升温,进样口温度为220℃,检测器为氢火焰离子化检测器,检测器温度为250℃,载气为氮气,载气流速为2.0 mL/min,分流比为10∶1,顶空平衡温度为80℃,平衡时间为20 min,顶空进样量为1mL。结果:乙醇、丙酮、乙酸乙酯、N,N-二异丙基乙胺和甲苯检测质量浓度线性范围分别为10.0~501.4μg/mL(r=0.999 9)、10.0~501.4μg/mL(r=0.999 9)、10.1~502.6μg/mL(r=0.999 9)、0.2~11.4μg/mL(r=0.999 9)、1.8~89.4μg/mL(r=0.999 7);定量限分别为5.3、3.4、5.2、6.1、20.4μg/mL,检测限分别为1.4、1.1、1.3、1.6、5.9μg/mL;精密度试验的RSD<4.0%,稳定性、重复性试验中只检出丙酮,其RSD<4.0%;加样回收率分别为96.61%~99.70%(RSD=1.01%,n=9)、95.81%~99.50%(RSD=1.29%,n=9)、96.42%~99.76%(RSD=1.24%,n=9)、96.36%~99.30%(RSD=1.19%,n=9)、97.00%~99.51%(RSD=0.82%,n=9)。结论:该方法简单、准确、重复性好,可用于法匹拉韦原料药中5种有机溶剂残留量的同时测定。 OBJECTIVE: To establish a method for simultaneous determination of 5 kinds residual ethanol, acetone, ethylace- tate, N, N-diisopropylethylamine and toluene in favipiravir. METHODS: Headspace GC was adopted. The determination was per- formed on DB-624 capillary column, temperature programmed. The inlet temperature was 220 ℃, and detector was flame ioniza- tion detector with temperature of 250℃. Nitrogen was used as carrier gas at flow rate of 2.0 mL/min, split ratio was 10 : 1, head- space equilibrium temperature was 80 %, equilibrium time was 20 min and headspace sample size was 1 mL. RESULTS: The lin- ear range was 10.0-501.4 μg/mL for ethanol(r=0.999 9), 10.0-501.4 μg/mL for acetone(r=0.999 9), 10.1-502.6 μg/mL for ethyl- acetate (r = 0.999 9 ) , 0.2-11.4 μg/mL for N, N-diisopropylethylamine ( r = 0.999 9) and 1.8-89.4μg/mL for acetone (r----0.999 7). The limits of quantification were 5.3, 3.4, 5.2, 6.1 and 20.4 μg/mL, and the limits of detection were 1.4, 1.1, 1.3, 1.6, 5.9 μg/ mL. RSD of precision test was lower than 4.0%, and RSDs of acetone in stability and reproducibility tests were both lower than 4.0%. The recoveries were 96.61%-99.70% (RSD=l.01%, n=9), 95.81%-99.50% (RSD=1.29%, n=9), 96.42%-99.76% (RSD=l.24%, n=9), 96.36% -99.30% (RSD=1.19%, n=9), 97.00% -99.51% (RSD=0.82%, n=9). CONCLUSIONS: The method is simple, accurate, reproducible and can be used for simultaneous determination of 5 organic solvents in favipiravir.
出处 《中国药房》 CAS 北大核心 2017年第24期3415-3418,共4页 China Pharmacy
基金 山东省自然科学基金资助项目(No.ZR2013HQ043)
关键词 气相色谱法 法匹拉韦 有机溶剂 残留量 乙醇 丙酮 乙酸乙酯 N N-二异丙基乙胺 甲苯 Gas chromatography Favipiravir Organic solvents Residual Ethanol Acetone Ethylacetate N,N-diisopropyle-thylamine Toluene
  • 相关文献

参考文献10

二级参考文献57

共引文献141

同被引文献64

引证文献8

二级引证文献24

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部