几种二阶校正方法结合三维荧光测定中药中的有效组分

发布时间：2018-08-30 12:12

【摘要】：化学计量学是一门涉及数学、计算机科学和分析化学的交叉学科,用于从化学量测过程中最大限度地获取有用的化学信息。化学计量学的二阶校正法可以在未知干扰共存的情况下,以“数学分离”代替化学分离,直接对分析物进行定性与定量分析。中药是中国传统文化的优秀组成部分,有着悠久的历史。中药成分复杂,其药效组分大都具有荧光性质。本文运用三维荧光结合二阶校正法对中药和人体液中的药效组分进行直接解析。第二章将交替三线性分解算法(ATLD)和三维荧光结合,对中药徐长卿和丹皮酚软膏中丹皮酚的含量及回收率进行了测定。徐长卿和丹皮酚软膏中都存在背景干扰成分,并且干扰成分的荧光光谱与丹皮酚的荧光光谱发生重叠。采用二阶校正法对三维荧光数据进行直接解析,避免了化学分离步骤,得到定性与定量分析结果,并且用高效液相色谱法进行了验证,结果比较满意。第三章研究了中药石菖蒲和南鹤虱中α-细辛醚和β-细辛醚的含量。α-细辛醚和β-细辛醚荧光性质十分相似,光谱重叠严重,单纯的荧光分析法很难同时测定这两种组分。运用三维荧光结合二阶校正法可以对石菖蒲和南鹤虱中α-细辛醚和β-细辛醚的含量直接进行解析。比较了平行因子分析法(PARAFAC)、交替三线性分解法(ATLD)、自加权交替三线性分解法(SWATLD)、交替惩罚三线性分解法(APTLD)、展开偏最小二乘-残差双线性分解法(U-PLS/RBL)和多向偏最小二乘-残差双线性分解法(N-PLS/RBL)这六种二阶校正法的解析结果,并且用高效液相色谱法进行验证,发现U-PLS/RBL和N-PLS/RBL法在α-细辛醚和β-细辛醚含量测定中具有一定的优势,得到的结果更加准确。分别用U-PLS/RBL法和N-PLS/RBL法对石菖蒲和南鹤虱中α-细辛醚、β-细辛醚回收率进行了解析,回收率良好。第四章比较了六种二阶校正法对血浆和尿液中α-细辛醚的浓度进行测定,并且比较了α-细辛醚浓度高和浓度低时的测定结果。血浆和尿液中都存在一种背景干扰成分,α-细辛醚浓度低时干扰更严重。用二阶校正法可以不经分离直接测定待测物浓度,六种二阶校正法得到的结果基本一致,回收率良好。
[Abstract]:Chemometrics is an interdisciplinary discipline involving mathematics, computer science and analytical chemistry, which is used to maximize the availability of chemical information from the chemical measurement process. The second-order calibration method of chemometrics can replace chemical separation with "mathematical separation" in the presence of unknown interference, and directly carry out qualitative and quantitative analysis of the analyte. Chinese traditional medicine is an excellent part of Chinese traditional culture, with a long history. The composition of traditional Chinese medicine is complex, and most of its active components have fluorescence properties. In this paper, the three dimensional fluorescence and second order correction method were used to analyze the pharmacodynamic components of traditional Chinese medicine and human body liquid. In chapter 2, the content and recovery of paeonol in traditional Chinese medicine Xu Changqing and paeonol ointment were determined by combining alternating trilinear decomposition algorithm (ATLD) with 3D fluorescence. Background interference was found in both Hsu Changqing and paeonol ointment, and the fluorescence spectra of interference components overlapped with those of paeonol. The second order correction method is used to analyze the three dimensional fluorescence data directly, avoiding the chemical separation step, and the qualitative and quantitative results are obtained. The results are verified by high performance liquid chromatography (HPLC), and the results are satisfactory. In the third chapter, the contents of 伪 -asarone and 尾 -asarone in Acorus calamus and Acanthophora chinensis were studied. The fluorescence properties of 伪 -asarone and 尾 -asarone are very similar, and the spectrum overlap is serious. It is difficult to determine these two components simultaneously by fluorescence analysis alone. The content of 伪-asarone and 尾-asarone in Acorus calamus and Crapa chinensis can be directly analyzed by using three dimensional fluorescence and second order correction method. The parallel factor analysis method (PARAFAC), alternating trilinear decomposition method (ATLD), self-weighted alternating trilinear decomposition method (SWATLD), alternating penalty trilinear decomposition method (APTLD), expansion partial least-squares bilinear decomposition method (U-PLS/RBL) and multidirectional partial least squares residual method are compared. The analytical results of the six second-order correction methods called differential bilinear decomposition (N-PLS/RBL), The method of U-PLS/RBL and N-PLS/RBL has some advantages in the determination of 伪 -asarone and 尾 -asarone, and the results obtained are more accurate. The recoveries of 伪 -asarone and 尾 -asarone in Acorus calamus and Cladopper chinensis were analyzed by U-PLS/RBL method and N-PLS/RBL method, respectively, and the recoveries of 伪 -asarone and 尾 -asarone were good. In chapter 4, six second-order calibration methods are compared to determine the concentration of 伪 -asarone in plasma and urine, and the results are compared when the concentration of 伪 -asarone is high or low. There is a background interference component in both plasma and urine, especially when 伪-asarone concentration is low. The second order correction method can be used to directly determine the concentration of the object to be measured without separation. The results obtained by the six two order correction methods are basically the same and the recovery rate is good.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R284.1;O657.3

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