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作 者:孙汉文[1] 问海芳[1] 苏明[1] 李丽清[1,2]
机构地区:[1]河北大学化学与环境科学学院河北省分析科学技术实验室,河北保定071002 [2]泰山学院化学系,山东泰安271021
出 处:《分析测试学报》2009年第2期168-172,共5页Journal of Instrumental Analysis
基 金:教育部博士点学科基金资助项目(20050075003);河北省自然科学基金资助项目(B2008000583)
摘 要:建立了毛细管电泳-电致化学发光同时测定丁卡因和普鲁卡因的新方法。考察了毛细管电泳流动相和检测池中磷酸盐缓冲液pH和浓度、进样时间和电压、分离电压和检测电位等对丁卡因和普鲁卡因的分离以及联吡啶钌电致化学发光检测的影响。基于循环伏安法考察了丁卡因和普鲁卡因的电化学行为与发光机理。在优化的实验条件下,丁卡因和普鲁卡因的标准曲线分别在6.6~265.6μmol/L和0.7~219.0μmol/L范围内呈良好的线性,检出限(S/N=3)分别为1.9μmol/L和0.2μmol/L。对23μmol/L丁卡因和15μmol/L普鲁卡因的标准溶液连续测定5次,迁移时间的相对标准偏差(RSD)分别为0.13%、0.16%,电化学法发光强度的RSD分别为3.7%和4.9%。该方法已成功用于血浆中丁卡因和普鲁卡因的同时检测,平均回收率均为94%,相对标准偏差低于4%。A new method was developed for simultaneous determination of tetracaine and procaine in human plasma by capillary electrophoresis ( CE ) with electrochemiluminescence (ECL) detection. The effects of experimental conditions, such as pH value, buffer concentration, injection time and voltage on the capillary electrophoresis separation and [ Ru (bpy)^2+ 3] electrochemiluminescence signal were investigated and optimized in detail. The electrochemical behavior of tetracaine and procaine, and electrochemiluminescence mechanism were investigated by cyclic voltammetric method. Under the optimum experimental conditions, the calibration curves for tetracaine and procaine showed a good linearity in the range of 6.6 -265.6 μmol/L and 0. 7 -219.0 μmol/L, and the limits of detection (S/N =3 ) were 1.9 I.~mol/L and 0.2 μmol/L, respectively. The relative standard deviations (RSDs) obtained by five measurements of 23 μmol/L tetracaine and 15 μmol/L procaine were 0. 13% and 0. 16% for the migration time, and 3.7% and 4.9% for the emission intensity, respectively. The proposed method was successfully applied to determine tetracaine and procaine in human plasma with average recoveries of 94% for both of them and RSDs of less than 4% .
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