Perrett D, Ross G A
Department of Medicine, St. Bartholomew's Hospital Medical School, West Smithfield, London, UK.
J Chromatogr A. 1995 May 12;700(1-2):179-86. doi: 10.1016/0021-9673(95)00101-r.
A micellar electrokinetic capillary chromatography method was developed that permitted the resolution of antipyrine from endogenous compounds and its quantitation in neat saliva in as little as 1 min. Final conditions were: SpectraPhoresis 1000, 30(23) cm x 50 microns silica capillary, 50 mM sodium phosphate pH 9.6, 50 mM SDS, 10 s hydrodynamic load, detection scanning 200-300 nm or 260 nm, run 25 kV. To overcome the effects of Joule heating the capillary was cooled to 15 degrees C. Sensitivity was < 10 microM and linearity extended to 350 microM. Comparison with an HPLC assay demonstrated that hydrodynamic injection gave a loading bias unless samples and standards were of equal viscosity. For 75 samples from five subjects the correlation of CE vs. HPLC was then r = 0.99.
开发了一种胶束电动毛细管色谱法，该方法能够在短短1分钟内从内源性化合物中分离出安替比林并对纯唾液中的安替比林进行定量分析。最终条件为：SpectraPhoresis 1000，30(23)厘米×50微米硅胶毛细管，50 mM磷酸钠（pH 9.6），50 mM十二烷基硫酸钠，10秒水力进样，检测扫描波长200 - 300纳米或260纳米，运行电压25 kV。为克服焦耳热的影响，将毛细管冷却至15摄氏度。灵敏度小于10微摩尔，线性范围扩展至350微摩尔。与高效液相色谱法测定结果的比较表明，除非样品和标准品的粘度相同，否则水力进样会产生进样偏差。对于来自五名受试者的75个样品，毛细管电泳与高效液相色谱法的相关性r = 0.99。
