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

采用熔融石英毛细管,以含有50 mmol/L 十二烷基硫酸钠的50 mmol/L硼酸盐缓冲液为电极缓冲液,以10 mmol/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sweeping(推扫)富集技术检测中性脂溶性物质旋覆花内酯(acetylbritannilactone,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0.005 g/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0.9975。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sweeping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。

Detection of Acetylbritannilactone in Inulicin Ingredients and Dynamic Change in Vivo by Micellar Electrokinetic Capillary Chromatography

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) x 75 microm 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 10 mmol/L borate buffer (pH 9.5). Other conditions were as follows: separation voltage, 23 kV; detection wavelength, 195 nm; sample injection, 3.45 kPa (0.5 psi) x 5 s; column temperature, 25 degrees C. 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 micro-amount of samples, and is characterized by higher degree of automation and sensitivity.