大口径石英毛细管柱气相色谱法测定黄豆甙原中有机溶剂残留量  

Capillary Column Gas Chromatographic Determination of Residual Solvents in Daidzein

作　　者：孙心齐[1] 王超杰[1] 赵文善[1] 

机构地区：[1]河南大学化学化工学院,开封475001

出　　处：《理化检验（化学分册）》2008年第9期846-847,850,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：用毛细管气相色谱法测定黄豆甙原中有机溶剂残留量。试样0.5g溶于含有内标正丁醇的二甲亚砜中,定容5mL。在优化条件下,用配有DB-17石英毛细管分离柱(0.54mm×30m,1.0μm)和火焰电离检测器的毛细管柱气相色谱仪测定黄豆甙原中残留的有机溶剂乙醇和N,N-二甲基甲酰胺(DMF)。乙醇和DMF的检出限分别是9.6pg和5.7ng;回归方程和相关系数分别为Y=0.04627+0.65369X,r=0.9982和Y=0.02531+0.35654X,r=0.9934;线性范围分别为50.4～718.9g·L^(-1)和9.8～137.2g·L^(-1)。A method of capillary column gas chromatography for the determination of residual solvents in daidzein was reported in this paper. The sample （0. 5 g） was dissolved in DMSO containing n-butanol as internal standard and made up to volume of 5 mL. Under the optimized conditions, using a gas chromatograph equipped with DB-17 quartz capillary column （0. 54 mm×30 m, 1.0μm） as separation column and FID as detector, the residual solvents, ethanol and DMF, in daidzein were determined. Detection limits were 9. 6 pg for ethanol and 5.7 ng for DMF. Linear regression equations were Y = 0. 046 27 ＋ 0. 653 69 X with r = 0. 998 2 for ethanol, and Y = 0. 025 31 X＋0. 356 54 X with r=0. 993 4 for DMF. Linearity was ranged in 50. 4--718. 9 g · L^-1 for ethanol and 9.8--137.2 g · L^-1 for DMF.

关 键 词：毛细管气相色谱 黄豆甙原 有机溶剂 

分 类 号：O657.7[理学—分析化学]