在线推扫富集-胶束电动毛细管色谱检测旋覆花素中和大鼠血浆中的旋覆花内酯  

Determination of Acetylbritannilactone in Inulicin and Rat Plasma by Micellar Electrokinetic Capillary Chromatography with On-Line Sweeping Concentration Technique

作　　者：赵京山[1] 温进坤[1] 韩梅[1] 

机构地区：[1]河北医科大学基础医学研究所河北省医学生物技术重点实验室,河北石家庄050017

出　　处：《色谱》2006年第5期508-512,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(No.30270499);河北省自然科学基金资助项目(No.303454)

摘　　要：采用熔融石英毛细管,以含有50mm o l/L十二烷基硫酸钠的50mm o l/L硼酸盐缓冲液为电极缓冲液,以10mm o l/L硼酸盐缓冲液为上样缓冲液,经过对分离条件的优化,成功地建立了胶束电动毛细管色谱结合在线sw eep ing(推扫)富集技术检测中性脂溶性物质旋覆花内酯(acety lb ritann ilac tone,ABL)的实验方法。所建方法的批内、批间测定值的相对标准偏差均小于5%,灵敏度为0.005g/L,回收率大于92%;被检测样品的含量与峰面积呈良好的线性关系,相关系数为0.997 5。用所建立的方法检测了旋覆花素中ABL的含量及其在体内的动态变化,结果表明胶束电动毛细管色谱结合在线sw eep ing样品富集技术可显著提高检测的灵敏度。该方法具有操作简单、进样量小(nL级)、检测速度快等特点,弥补了毛细管电泳在测定痕量组分方面的不足。A method was established for the determination of acetylbritannilactone （ABL） in inulicins and rat plasma by micellar electrokinetic capillary chromatography （MECC）, in which on-line sweeping technique was applied to elevate the sensitivity of the detection. The column used was an uncoated fused silica capillary with a size of 57 cm （effective length of 50 cm） × 75 p.m i.d. Electrode buffer was a 50 mmol/L borate buffer containing 50 mmol/L sodium lauryl sulfate （SDS） （pH 9.5）. Sample buffer was a l0 mmol/L borate buffer （pH 9.5）. Other conditions were as follows： separation voltage, 23 kV; detection wavelength, 195 rim; sample injection, 3.45 kPa （0.5 psi） × 5 s; column temperature, 25 ℃. The on-line sweeping-MECC had excellent linearity with correlation coefficient of 0. 997 5, and reproducibility with the relative standard deviation of ABL migration time less than 5%. The recovery was more than 92%, and the sensitivity was 0. 005 g/L. ABL in inulicin and their dynamic change in vivo were determined by sweeping-MECC. The results indicate that on-line sweeping-MECC is a simple and rapid method for the determination of trace biological sample. The method needs only microamount of samples, and is characterized by higher degree of automation and sensitivity.

关 键 词：胶束电动毛细管色谱 sweeping在线富集技术 旋覆花内酯 旋覆花素 大鼠血浆 

分 类 号：O658[理学—分析化学]