研究用芯片毛细管电泳激光诱导荧光检测系统分离测定经7-chloro-4-nitrobenzo-2-oax-1,3-diazole(NBD-Cl)衍生的麻黄碱和伪麻黄碱的实验条件。采用胶束毛细管电动色谱分离体系(12mmol/L SDS+10mmol/L硼砂缓冲液,pH9.0),在45mm长的通道上实现了麻黄碱和伪麻黄碱的快速分离,一次分离小于1.5min。10—100ms/L范围内,峰高与浓度呈良好的线性关系,麻黄碱、伪麻黄碱的检出限分别是0.83mg/L和1.10mg/L。所建立的方法应用于尿中麻黄碱和伪麻黄碱的分离测定,取得满意的结果。
A method was developed for the determination of ephedrine (EP) and pseudoephedrine (PEP) dopes in urine with a chip-based capillary electrophoresis and laser induced fluorescence detector system ( CELIF). The dopes were derived with 7-chloro-4nitrobenzo-2-oax-1,3-diazole (NBD-Cl) to form fluorescent products. By using a separation channel of 45 mm in length, various experimental conditions for CE separation were optimized, and a separation mode of micellar capillary electrokinetic chromatography was adopted. Under the optimized conditions (12 mmol/L sodium dodecyl sulfonate (SDS) + 10 mmol/L tetraborate buffer at pH 9.0, 2600V separation voltage), EP and PEP can be base-line separated from the reagent components as well as the species existing in the urine within 1.5 min. A linear calibration curve was observed in the concentrations ranging from 10 to 100 mg/L for both EP and PEP, the limits of detection obtained were 0.83 mg/L for EP and 1.10 mg/L for PEP. Satisfactory recoveries were achieved when the developed method was used for determination of EP and PEP concentration spiked into human urine.