Zhou Min, Ma Yong-Jun, Ren Xiao-Na, Zhou Xiu-Ying, Li Li, Chen Hui
Gansu Key Laboratory of Polymer Materials, College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070, China.
Anal Chim Acta. 2007 Mar 21;587(1):104-9. doi: 10.1016/j.aca.2007.01.018. Epub 2007 Jan 16.
A Ru(bpy)(3)(2+)-based electrochemiluminescence (ECL) detection coupled with capillary electrophoresis (CE) has been established for the determination of sinomenine for the first time. Optimum separation was achieved with a fused-silica capillary column (50 cm x 25 microm i.d.) and a background electrolyte of 50 mM sodium phosphate (pH 5.0) at a separation voltage of 15 kV. The content of sinomenine was detected by ECL at the detection voltage of 1.15 V (versus Ag/AgCl) with 5 mM Ru(bpy)(3)(2+) in 75 mM phosphate solution (pH 8.0) when a chemically modified platinum electrode by europium(III)-doped prussian blue analogue (Eu-PB) was used as a working electrode. Under the optimized conditions, the ECL intensity was in proportion to sinomenine concentration in the range from 0.01 to 1.0 microg mL(-1) with a detection limit of 2.0 ng mL(-1) (3sigma). The relative standard derivations of migration time and ECL intensity were 0.93 and 1.11%, respectively. The level of sinomenine in Sinomenium acutum Rehd. et Wils was easily determined with recoveries between 98.6 and 102.7%.
首次建立了基于钌(联吡啶)(3)(2 +)的电化学发光(ECL)检测与毛细管电泳(CE)联用的方法来测定青藤碱。使用熔融石英毛细管柱(50 cm×25μm内径),以50 mM磷酸钠(pH 5.0)为背景电解质,在15 kV的分离电压下实现了最佳分离。当使用铕(III)掺杂普鲁士蓝类似物(Eu-PB)化学修饰的铂电极作为工作电极时,在1.15 V(相对于Ag/AgCl)的检测电压下,用ECL检测青藤碱的含量,检测溶液为含5 mM钌(联吡啶)(3)(2 +)的75 mM磷酸盐溶液(pH 8.0)。在优化条件下,ECL强度与青藤碱浓度在0.01至1.0μg mL(-1)范围内成正比,检测限为2.0 ng mL(-1)(3σ)。迁移时间和ECL强度的相对标准偏差分别为0.93%和1.11%。该方法可轻松测定青风藤中青藤碱的含量,回收率在98.6%至102.7%之间。