[关键词]
[摘要]
建立了沸水浴去血清蛋白质后用HPLC直接测定阿魏酸(FA)方法:方剂的血样预处理新方法分别用二维、三维HPLC和分光光度计定性测定FA后,用内标(香豆精)法定量。甲醇-乙酸-水(38:0.3:61.7)为流动相,C18(ODS2)柱(150mm×4.6mm,5μm)为固定相时,FA的最低检测限6ng;沸水浴10min的最低检测血清浓度是20.2ng/ml,线性范围33.7~2156.8ng/ml=0.9993;方法平均回收率(93.59±1.93)%,日间及日内精密度RSD值均为8.44%。上法已用于人服川芎汤后经时变化的血清FA浓度测定。
[Key word]
[Abstract]
A new method for the determination of ferulic acid in serum samples after oral administration of TCM by HPLC has been developed. Serum samples containing ferulic acid (FA)and internal standard coumarin (IS) were first treated in boiling water-bath to deproteinate,and the FA and IS in the supernant analysed by 2D, 3D HPLC and spectrometry, on C18 column (150 mm X 4. 6 mm,5 }cm,)with MeOH:HOAc:H2O (38:0. 3:61. 7) as the mobile phase,and detected at 320 nm. Results showed that (1)the minimal detectable limits of blank methanol and serum concentrations of FA were 6 ng and 20. 6 ng/mL;(2) the linearity ranged from 33.7 to 2 156. 8 ng/mL (r=0. 9993);(3) the mean recovery was 93. 59士 1. 93;and (4) RSD of within day and day to day were less than 8. 4400" In a pilot study, serum samples collected from healthy volunteers following oral administration of a decoction of Chuanxiong (Ligusticum chuanxiong Hort.)gave a concentration-time curve of FA with accurate and reproducible results.
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[基金项目]
国家自然科学基金项目39100139;39570870;39670865;39870932;博士后基金(96)4