蚕沙生物碱提取物中乙醇残留量的测定  

Determination of Residual Organic Solvents in Alkaloid Extract of Silkworm

作　　者：赵辉[1] 李琳[1] 丁振营[1] 亓晖[1] 白钢[1] 朱元元[1] 

机构地区：[1]南开大学药学院,天津市分子药物研究重点实验室,天津300071

出　　处：《南开大学学报（自然科学版）》2012年第2期110-112,共3页Acta Scientiarum Naturalium Universitatis Nankaiensis

基　　金：国家重大科技专项(2009ZX09103-363)

摘　　要：建立了蚕沙生物碱提取物中有机残留量的测定方法.采用直接进样毛细管气相色谱法,色谱柱是以100%2-甲基聚硅氧烷为固定相的石英毛细管柱Rtx-1(30 m×0.25 mm,0.25μm),以N,N-2甲基甲酰胺(DMF)为溶剂,载气为氮气,流速1.0 mL/min,采用氢离子火焰检测器(FID),检测器温度为350℃,进样口温度350℃,分流比30∶1,进样量1μL,柱温采用程序升温:初始温度为30℃,保持5 min,以80℃/min升温至110℃,保持5 min,再以60℃/min升温至320℃.被测物在0.004～0.072 mg/mL范围内呈良好线性关系,回收率为100.3%.方法快速,准确可靠,可用于蚕沙生物碱提取物中有机溶剂残留的检测.A capillary gas chromatography methodology was estiblised for the determination of ethanol in alkaloid extraction of silkworm. A capillary gas chromatographic method with directly sampling was employed. The analytical column was Rtx-1（30 m × 0.25 mm, 0. 25 μm）. The samples were dissolved in DMF. The column temperature was programmed. The carrier gas was nitrogen and its flow-rate was 1.0 mL/min. The detector was FID and its temperature was 350 C. The injector temperature was 350 C, the split ratio was 30： 1, and the injection volume was 1 μL. The linear range of ethanol was from 0. 004 to 0. 072 mg/L. The average recovery from sample was 100. 3%. The method is simple,rapid,specific and precise. It could be used for the determination of residual amounts of ethanol in drug substances.

关 键 词：蚕沙生物碱提取物 毛细管气相色谱 乙醇 残留量 DMF 

分 类 号：R927.11[医药卫生—药学]