尿液中麻黄碱与可待因的扫集胶束电动色谱法快速测定  被引量:5

Rapid Determination of Ephedrine and Codeine in Human Urine by Sweeping Micellar Electrokinetic Chromatography

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作  者:李利军[1] 李斯光[2] 蔡卓[2] 李丽娜[2] 程昊[1] 

机构地区:[1]广西工学院生物与化学工程系,广西柳州545006 [2]广西大学化学与化学工程学院,广西南宁530004

出  处:《分析测试学报》2008年第12期1359-1362,共4页Journal of Instrumental Analysis

基  金:广西自然科学基金资助项目(桂科自0481019)

摘  要:采用扫集胶束毛细管电泳,建立了快速测定尿液中麻黄碱和可待因含量的方法,并通过日内、日间实验对方法的稳定性进行考察。讨论了pH值、十二烷基硫酸钠(SDS)浓度、分离电压、进样时间等因素的影响。建立了扫集胶束电动色谱的最佳实验条件,其中pH 2.2缓冲体系含80 mmol/L SDS,20 mmol/LNaH2PO4,18%(体积分数)乙腈,分离电压-20 kV,测量波长200 nm。在优化条件下,麻黄碱和可待因均在7 min内出峰,方法检出限(mg/L)、线性范围(mg/L)、相关系数分别为麻黄碱0.173、0.693-11.1、0.9993,可待因0.333、1.33-16.0、0.9993,应用于实际样品测定,回收率为94%-108%,RSD不大于3.5%。峰面积日内RSD不大于6.3%(n=5),日间RSD不大于9.3%(n=5)。The sweeping micellar electrokinetic chromatography ( Sweeping - MEKC ) method was developed for the determination of ephedrine(Ep) and codeine(Co) in human urine sample. Stability of this method was evaluated by intra-day and inter-day experiments. The effects of pH, SDS concentration, separation voltage and injection time on the separation efficiency were discussed. The optimal conditions were using pH 2.2 20 mmoL/L NaH2PO4 as buffer containing 80 mmol/L SDS, and 18% ACN ( by volume) , applying separation voltage of - 20 kV and reading at 200 nm. Under the optimal conditions, the separation of Ep and Co was finished in 7 min. The LODs (mg/L), linearity( mg/ L) and correlation coefficient were 0. 173, 0. 693 - 11.1 and 0. 999 3 for Ep, 0. 333, 1.33 - 16. 0 and 0. 999 3 for Co, respectively. The RSDs of peak areas were no more than 6.3% for intra-day(n = 5 ) and 9.3% for inter-day( n = 5 ). This method was successfully used in the determination of Ep and Co of human urine with recoveries of 94% - 108% , and RSD of no more than 3.5%.

关 键 词:扫集胶束电动色谱法 麻黄碱 可待因 

分 类 号:O657.8[理学—分析化学] R446.12[理学—化学]

 

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