U-PLS/RBL三维荧光法测定藤络宁胶囊中东莨菪内酯含量
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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 p H 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 between310 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.
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 p H 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 between310 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.
引文
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[3]Song W,Jin R L,Liu J H.Chin.J.Chin.Mater.Med.(宋蔚,金蓉鸾,刘继华.中国中药杂志),1997,22(6):359-360.
[4]Chen Z,Liao L,Zhang Z,Wu L,Wang Z.J.Ethnopharmacol.,2013,150(2):501-506.
[5]Moon P D,Lee B H,Jeong H J,An H J,Park S J,Kim H R,Ko S G,Um J Y,Hong S H,Kim H M.Eur.J.Pharmacol.,2007,555:218-225.
[6]Kim H J,Jang S I,Kim Y J,Chung H T,Yun Y J,Kang T H,Jeong O S,Kim Y C.Fitoterapia,2004,75:261-266.
[7]Pan R,Dai Y,Gao X,Dan L,Xia Y.Vasc.Pharmacol.,2011,54:18-28.
[8]Cao H,Qin H L,Zhong X F,Liu Y.Chin.Pharm.J.(曹红,秦红霖,钟晓峰,刘云.中国药学杂志),2001,6:411-414.
[9]Mu1oz de la Pe1a A,Goicoechea H C,Escandar M G,Olivieri A C.Fundamentals and Analytical Applications of Multiway Calibrations.Waltham:Elsevier,2015.
[10]Yin X L,Wu H L,Zhang X H,Gu H W,Yu R Q.Aata Chim.Sin.(尹小丽,吴海龙,张晓华,谷惠文,俞汝勤.化学学报),2013,71:560-566.
[11]Yang L,Liu D L,Wei Y J.J.Instrum.Anal.(杨莉,刘德龙,魏永巨.分析测试学报),2014,33(9):1038-1043.
[12]Wu H L,Li Y,Kang C,Yu R Q.Chin.J.Anal.Chem.(吴海龙,李勇,康超,俞汝勤.分析化学),2015,43(11):1038-1043.
[13]Calimag-Williams K,Knobel G,Goicoechea H C,Campiglia A D.Anal.Chim.Acta,2014,811:60-69.
[14]Bravo M A,Escandar G M,Olivieri A C,Bardin E,Aguilar L F,Quiroz W.Chemom.Intell.Lab.Syst.,2015,148:77-84.
[15]Hurtado-Sánchez M D,Lozano V A,Rodríguez-Cáceres M I,Durán-Merás I,Escandar G M.Talanta,2015,134:215-223.
[16]Alarcon F,Baez M E,Bravo M,Richter P,Escandar G M,Olivieri A C,Fuentesa E.Talanta,2013,103:361-370.
[17]Vidal R B,Iba1ez G A,Escandar G M.Talanta,2015,143:162-168.
[18]Bortolato S A,Arancibia J A,Escandar G M.Environ.Sci.Technol.,2011,45:1513-1520.
[19]Cabrera-Ba1egil M,Hurtado-Sánchez M D,Galeano-Díaz T,Durán-Merás I.Food Chem.,2017,220:168-176.
[20]Haaland D M,Thomas E V.Anal.Chem.,1988,60:1193-1202.