毛细管电泳电化学发光法测定蜂蜜中土霉素残留量  

Determination of Oxytetracycline Residue in Honey by Capillary Electrophoresis and Electrochemiluminescent Detection

作　　者：赵红岩[1] 蔡诚[1] 王园朝[1] 

机构地区：[1]杭州师范大学材料与化学化工学院,浙江杭州310036

出　　处：《分析测试学报》2015年第5期576-581,共6页Journal of Instrumental Analysis

基　　金：浙江省科技厅公益计划项目(2012C37011)

摘　　要：基于土霉素对联吡啶钌（Ru（bpy）2＋3）的电化学发光（ECL）信号的增强效应,建立了毛细管电泳-电化学发光法（CE-ECL）测定土霉素的新方法。利用场放大效应将检测灵敏度提高了3.5倍,最佳检测电位为1.22 V,运行缓冲液为8 mmol·L-1硼砂溶液（p H 8.0）,进样时间及电压分别为6 s和10 k V。在优化条件下,土霉素可在9 min内检出,其线性范围为20~200μg·L-1,相关系数为0.995 3,仪器检出限（S/N=3）为5μg·L-1;5次测定100μg·L-1土霉素溶液的ECL信号和迁移时间的日内重现性分别为2.4%和2.1%,日间重现性分别为3.6%和2.8%。方法用于市售蜂蜜中土霉素残留的测定,在200,1 000,2 000μg·kg-1加标浓度下的回收率为91.5%~105.2%。方法检出限（LOD,S/N=3）为10μg·kg-1,低于食品中土霉素的最大残留限值（MRL）。结果表明该方法在食品分析中具有一定的应用价值。A novel method was proposed for the determination of oxytetracycline by capillary electrophoresis（ CE） with electrochemiluminescent（ ECL） detection based on the enhancement effect of ECL intensity in the tris（ 2,2＇-bipyridine）-ruthenium（ Ⅱ）（ Ru（ bpy）2 ＋3-ECL） system by oxytetracycline. The sensitivity was further improved by 3. 5-fold by the field amplified sample injection technique. The best result was achieved with a sampling voltage of 10 k V and an injection time of 6 s in8 mmol·L-1borate buffer（ p H 8. 0） at a detection voltage of 1. 22 V. The consumed time for one run was about 9 min. A linear range of 20-200 μg·L-1（ r = 0. 995 3） with a limit of detection（ S /N = 3） of 5 μg·L-1was obtained by the proposed method. The intra-day relative standard deviations（ RSDs） of relative ECL intensity and migration time for five replicated trials of 100 μg·L-1oxytetracycline were 2. 4% and 2. 1%,respectively,and the inter-day RSDs of relative ECL intensity and migration time for five replicated trials of 100 μg ·L-1oxytetracycline were 3. 6% and 2. 8%,respectively. The developed method was successfully applied in the detection of oxytetracycline residue in a honey sample. The average recoveries were in the range of 91. 5%-105. 2% at spiked levels of200,1 000,2 000 μg·kg-1. The limit of detection for the proposed method was 10 μg·kg-1in honey matrix,which was lower than the maximum residue limit of oxytetracycline in food. The results indicated that the proposed method had an application potential in food analysis.

关 键 词：毛细管电泳电化学发光 联吡啶络钌 土霉素 蜂蜜 

分 类 号：O657.1[理学—分析化学] R978.1[理学—化学]