毛细管电泳-电致化学发光法分离测定麻黄中的麻黄碱、伪麻黄碱与甲基麻黄碱  

Separation and Determination of Ephedrine,Pseudoephedrine and Methylephedrine by Capillary Electrophoresis with Electrochemiluminescence Detection

作　　者：马永钧[1] 李琼琳[1] 王伟峰[1] 周敏[1] 何春晓[1] 刘婧[1] 

机构地区：[1]西北师范大学化学化工学院甘肃省生物电化学与环境分析重点实验室,甘肃兰州730070

出　　处：《分析测试学报》2012年第2期127-132,共6页Journal of Instrumental Analysis

基　　金：甘肃省自然科学基金资助项目(096RJZA117)

摘　　要：以PB-Eu化学修饰电极为工作电极,对乙烯基苄基三乙基氯化铵离子液体为拆分添加剂,首次采用毛细管电泳-电致化学发光法对麻黄碱、伪麻黄碱和甲基麻黄碱进行了分离和检测。考察了检测电位、分离缓冲液的种类和酸度、添加剂用量等条件对电泳分离效果及检测灵敏度的影响。在优化条件下,3种混合药物可在8 min内达到基线分离,甲基麻黄碱、麻黄碱和伪麻黄碱的质量浓度分别在0.025～10、0.025～25、0.05～10 mg/L范围内与其峰面积呈良好但斜率略不同的两区段型线性关系,总的线性响应范围可达3个数量级。以质量浓度均为1.00 mg/L的3种混合药物合成样品进行6次平行测试,其峰面积和迁移时间的RSD分别小于4.5%和0.95%。该方法成功用于商品麻黄碱类药物制剂及中药麻黄原药中3种生物碱含量的测定,加标回收率为101%～111%。Using an ionic liquid of p-vinylbenzyltriethylammonium chloride as separating additive,a novel method for the simultaneous determination of methylephedrine（ME）,ephedrine（E） and pseudoephedrine（PE） was developed by capillary electrophoresis coupled with electrochemiluminescence detection using PB-Eu chemically modified electrode as working electrode.The effect factors,such as detection potential,types and acidity of separation buffer on the separation efficiency were investigated.Under the optimized conditions,three analytes were separated well in 8 min.Good relationships（r2≥0.999 1） between peak area and concentrations of analytes（ME：0.025-10 mg/L,E：0.025-25 mg/L,PE：0.05-10 mg/L） were established over three orders of magnitude.The synthetic samples containing three alkaloids in a level of 1.00 mg/L were determined.The RSDs of peak area and migration time were less than 4.5% and 0.95%,respectively.The method was successfully used in the determination of the three alkaloids in pharmaceutical preparations and Chinese herbal Ma-Huang with recoveries of 101%-111%.

关 键 词：毛细管电泳 电致化学发光 离子液体 生物碱 

分 类 号：O657.8[理学—分析化学] TQ460.72[理学—化学]