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作 者:刘铁 刘德龙[1] 魏永巨[1] LIU Tie;LIU De-long;WEI Yong-ju(College of Chemistry and Materials Science,Hebei Normal University,Shijiazhuang 050024,China)
机构地区:[1]河北师范大学化学与材料科学学院,河北石家庄050024
出 处:《分析测试学报》2018年第3期313-318,共6页Journal of Instrumental Analysis
基 金:国家自然科学基金资助项目(20975029;81173496)
摘 要:研究了东莨菪内酯的荧光性质和最佳实验条件,发现体系的最佳p H值为9.0,最大激发波长为375nm,最大发射波长为460 nm。在激发波长310~420 nm,发射波长400~550 nm范围内采集实际样本的三维荧光数据矩阵。采用二阶校正中的U-PLS/RBL(Unfolded partial least squares coupled to residual bilinearization)解析三维荧光数据阵,成功地测定了藤络宁胶囊中的东莨菪内酯含量。用U-PLS/RBL解析藤络宁胶囊中的东莨菪内酯含量,结果与HPLC方法一致,说明荧光解析法结果准确可靠。用U-PLS/RBL解析藤络宁胶囊样品的加标回收率为100.4%。相比于色谱方法,荧光方法具有操作费用低及绿色环保等优点。A method for the determination of scopoletin in Tengluoning capsule by three-dimensional fluorescence combined with unfolded partial least squares coupled to residual bilinearization(U-PLS/RBL)was developed.Experiments showed that scopoletin has a strong fluorescent signal.The optimum pH of the system was 9.0,the maximum excitation wavelength of scopoletin was 375 nm,and the maximum emission wavelength was 460 nm.Excitation-emission matrices(EEM)of Tengluoning capsule samples were obtained,recording emission between 400 nm and 550 nm,exciting between 310 nm and 420 nm,for the analysis of scopoletin.An effective second-order calibration method,U-PLS/RBL(unfolded partial least-squares coupled to residual bilinearization)was used to analyze the three-dimensional fluorescent data array,and the content of scopoletin was successfully determined.The predicted U-PLS/RBL concentrations were satisfactory compared with those obtained by high performance liquid chromatography with fluorescence detection.The average recovery by U-PLS/RBL was 100.4%,which indicated that the proposed method was reliable.Compared to chromatographic method,the fluorescent method has the advantages of low operating cost and pro-environment.
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