Dong Yuming, Chen Hongli, Chen Yonglei, Hui Yang, Chen Xingguo, Hu Zhide
Department of Chemistry, Lanzhou University, Lanzhou, China.
J Sep Sci. 2006 Aug;29(13):2049-55. doi: 10.1002/jssc.200600073.
A micellar electrokinetic capillary chromatography method with laser-induced fluorescence detection was developed for the analysis of epinephrine and dopamine after derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole. The optimum derivatization conditions were: 30 mM sodium borate (pH adjusted to 8.0 with 1.0 M HCl), reaction time 30 min at 60 degrees C. Baseline separation was achieved within 14 min with a running buffer composed of 10 mM sodium borate + 25 mM sodium dodecyl sulfate (pH adjusted to 9.5 with 0.1 M NaOH) and an applied voltage of 15 kV. Good linearity relationships (correlation coefficients: 0.9991 for epinephrine and 0.9985 for dopamine) between peak areas and concentrations of the analytes were obtained. The detection limits and quantification limits for epinephrine and dopamine were 0.0038 mg/L and 0.013 mg/L, and 0.065 mg/L and 0.020 mg/L, respectively. The method was applied to the analysis of the two compounds in two Chinese medicines with recoveries in the range of 92.6-108.7%.
建立了一种胶束电动毛细管色谱法,采用激光诱导荧光检测技术,用于分析经4-氯-7-硝基苯并-2-恶唑-1,3-二唑衍生化后的肾上腺素和多巴胺。最佳衍生化条件为:30 mM硼酸钠(用1.0 M HCl将pH调至8.0),在60℃下反应30分钟。使用由10 mM硼酸钠 + 25 mM十二烷基硫酸钠(用0.1 M NaOH将pH调至9.5)组成的运行缓冲液和15 kV的施加电压,在14分钟内实现了基线分离。分析物的峰面积与浓度之间具有良好的线性关系(相关系数:肾上腺素为0.9991,多巴胺为0.9985)。肾上腺素和多巴胺的检测限和定量限分别为0.0038 mg/L和0.013 mg/L,以及0.065 mg/L和0.020 mg/L。该方法应用于两种中药中这两种化合物的分析,回收率在92.6 - 108.7%范围内。