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.
出处
《色谱》
CAS
CSCD
北大核心
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)
