CAJ | 학술논문

目的建立水飞蓟素中3种有机溶剂残留量的顶空气相色谱测定方法.方法以H P-5弹性石英毛细管柱(30m×0.53mm,i.d,5.0μm),载气为氮气,采用氢火焰离子化检测器,进样口温度为180℃,检测器温度为250℃,柱温采用程序升温(40℃,保持6min,以15℃/min升至180℃,保持3min),流速为1.7mL/min,分流比为1∶10,采用甲醇作为内标物质,分别配制对照溶液及样品溶液,以二甲基亚砜为溶剂,采取顶空进样(85℃预热20min),进样体积为1.0mL.结果乙醇、丙酮、乙酸乙酯在各自对应的浓度范围内,其峰面积与浓度呈良好的线性关系,加样回收率(n=5)分别为98.30%(RSD=0.82%)、97.62%(RSD=1.1%)、96.89%(RSD=1.4%),精密度良好.结论本文所建立的气相色谱条件可同时测定水飞蓟素中的乙醇、丙酮、乙酸乙酯的含量,方法简单可靠.
목적건립수비계소중3충유궤용제잔류량적정공기상색보측정방법.방법이H P-5탄성석영모세관주(30m×0.53mm,i.d,5.0μm),재기위담기,채용경화염리자화검측기,진양구온도위180℃,검측기온도위250℃,주온채용정서승온(40℃,보지6min,이15℃/min승지180℃,보지3min),류속위1.7mL/min,분류비위1∶10,채용갑순작위내표물질,분별배제대조용액급양품용액,이이갑기아풍위용제,채취정공진양(85℃예열20min),진양체적위1.0mL.결과을순、병동、을산을지재각자대응적농도범위내,기봉면적여농도정량호적선성관계,가양회수솔(n=5)분별위98.30%(RSD=0.82%)、97.62%(RSD=1.1%)、96.89%(RSD=1.4%),정밀도량호.결론본문소건립적기상색보조건가동시측정수비계소중적을순、병동、을산을지적함량,방법간단가고.
Objective This paper reports a GC method for determination of ethanol,acetone,ethyl acetate in Silymarin. Method The analytical column was HP-5 (30m×0.53mm,i.d,5.0μm).The injector temperature was 180℃,and the detector temperature was 250℃.The column temperature was programmed raised.The carrier gas was nitrogen,and the solvent was dimethyl sulfoxide.Results The standard curve were linear respectively.The average recoveries and precisions were good as well.Conclusion This method was found to be sensitive and accurate and was useful in control the residual solvents in Silymarin.