场放大进样-胶束扫集法测定升麻中3种有机酸  

Determination of Three Organic Acids in Rhizoma Cimicifugae Foetidae by Capillary Electrophoresis Using Field-Amplified Sample Stacking and Sweeping Micellar Electrokinetic Chromatographic Technique

作　　者：李利军[1] 蔡卓[2] 李斯光[2] 吴峰敏[2] 李海燕[3] 陈昌东[2] 程昊[1] 吴健玲[2] 

机构地区：[1]广西工学院生物与化学工程系,柳州545006 [2]广西大学化学化工学院,南宁530004 [3]中山大学中山医学院,广州510080

出　　处：《分析化学》2008年第9期1261-1264,共4页Chinese Journal of Analytical Chemistry

基　　金：广西自然科学基金(No.0481019)资助项目

摘　　要：利用两种在线富集技术,对阿魏酸、异阿魏酸、咖啡酸同时测定的方法进行了研究。在胶束扫集的基础上,联用场放大进样,使富集倍数提高了约100倍;检出限降至4μg/L,线性范围向下延伸到10μg/L。胶束扫集电动色谱缓冲体系为90mmol/LSDS+20mmol/LNa2PO4(pH=2.20)+10%甲醇,分离电压20kV。进样电压10kV,进样时间21s,进水时间210s(H=20.0cm),测量波长214nm。讨论了SDS浓度、进样长度、进样电压等对分离效果的影响。在优化条件下,3种有机酸在14min内出峰,峰面积RSD≤3.8%。方法检出限(μg/L)、线性范围(μg/L)、相关系数分别为:阿魏酸4.0、10～400、0.9982;异阿魏酸4.0、10～400、0.9970;咖啡酸5.0、10～400、0.9980。回收率为83.9%～114.3%。Field amplified sample stacking （FASS） and sweeping micellar electrokinetic chromatography （FASS-Sweep-MEKC） was used for the determination of ferulic acid, isoferulicacid, and caffeic acid. Com- pare with the common sweeping method, the sensitivity was improved about 100 times by FASS-Sweep, the LODs was decreased to ~g/L level, and the linear range was extended to 10 ~g/L. The buffer medium con- tains 90 mmol/L SDS, 20 mmol/L Nail2PO4 （pH 2.20）, and 10% methanol（V/V）. Separation voltage was 20 kV, sample injection voltage was 10 kV, injection time was 21 s, water injection time was 210 s （H =20.0 cm）, detected at 214 nm. Those of effect of SDS concentration, sample injection time and injec- tion voltage were optimized. Under the optimum conditions, the determination time was within 14 minutes with RSDs of peak area less than 3. 8%. The calibration plots were linear in the range of 10 - 400 μg/L, r≥0. 9970, and the LODs were 4 μg/L for ferulic acid and isoferulic acid, 5 μg/L for caffeic acid. Further- more, this proposed FASS-sweeping-MEKC method was successful applied for the detection of the three organ- ic acids in rhizoma cimicifugae foetidae.

关 键 词：毛细管电泳 场放大进样 胶束扫集 阿魏酸 异阿魏酸 咖啡酸 

分 类 号：R284[医药卫生—中药学]