恒波长同步荧光光谱法测定人体尿液中氯波必利的研究  

Study on the Determination of Clebopride in Human Urine by Constant-wavelength Synchronous Fluorimetry

作　　者：罗娟娟[1] 马红燕[1] 马莹[1] 辛建伟[1] 王浩[1] 

机构地区：[1]延安大学化学与化工学院分析化学研究所,陕西延安716000

出　　处：《分析测试学报》2011年第5期553-557,共5页Journal of Instrumental Analysis

基　　金：陕西省教育厅专项科研基金资助项目(09JK821);延安市科技局科技计划资助项目(2008ks-20)

摘　　要：研究发现甲醛溶液可使氯波必利的荧光强度显著增强。在pH为6.6的Britton-Robinson(B-R)缓冲介质中,以恒波长差Δλ=30 nm进行同步荧光扫描,可消除人体尿液中内源性荧光物质的背景干扰,其同步特征峰的强度与氯波必利的质量浓度呈线性关系,据此建立了直接测定尿样中氯波必利的恒波长同步荧光分析方法,并对测定条件进行了优化。氯波必利的质量浓度在2.8×10-5～4.0×10-3 g/L范围内与荧光强度呈良好线性,相关系数为0.999 9,方法检出限(3S0/S)为1.1×10-5 g/L。对4.0×10-5 g/L的氯波必利平行测定11次的相对标准偏差为1.7%。该方法可用于实际尿样中氯波必利含量的直接测定,其回收率为95%～104%。A rapid,simple,accurate and selective synchronous fluorimetry method was developed for the determination of clebopride in human urine sample.The experiments indicated that clebopride has endogenous fluorophore,the fluorescence intensity was enhanced remarkably after adding formaldehyde.Because the emission spectra of clebopride and fluorescent substance of human urine were overlapped partially,clebopride couldn＇t be determined directly by the normal fluorimetric method.In order to eliminate effectively the background interference of human urine,the synchronous spectrum（Δλ=30 nm） was selected for the determination of clebopride.The experimental conditions affecting the fluorescence intensity of clebopride was optimized.Under the optimumal conditions,the fluorescence intensity was linearly proportional to the concentration of clebopride in the range of 2.8×10-5-4.0×10-3 g/L with a correlation coefficient of 0.999 9.The detection limit was 1.1×10-5 g/L.The relative standard deviation（RSD,n=11） for the determination of 4.0×10-5 g/L clebopride solution was 1.7%.The proposed method was applied in the determination of clebopride in human urine samples with recoveries of 95%-104%.

关 键 词：氯波必利 甲醛 尿样 同步荧光法 

分 类 号：O561.3[理学—原子与分子物理] TQ460.72[理学—物理]