三维荧光二阶校正法快速测定人尿样中奥沙普秦含量  

Rapid Determination of Oxaprozin Contents in Urine and Combined Pharmacotherapy Samples Using Three-dimensional Fluorescence Coupled with Second-order Calibration Methods

作　　者：于丽丽[1] 吴海龙[1] 付海燕[1] 于永杰[1] 刘亚娟[1] 卿湘东[1] 俞汝勤[1] 

机构地区：[1]湖南大学化学化工学院,化学生物传感与计量学国家重点实验室,长沙410082

出　　处：《分析化学》2011年第1期27-33,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20775025);教育部创新团队项目资助

摘　　要：利用三维荧光光谱技术,结合分别基于自加权交替三线性分解(SWATLD)和交替归一加权残差(ANWE)算法的二阶校正方法,直接快速测定人体样液中以及萘丁美酮或萘普生干扰共存下奥沙普秦的含量。利用本方法的"二阶优势",在尿液内源物质及萘丁美酮或萘普生干扰共存下有效地分辨出奥沙普秦的激发发射荧光光谱。采用SWATLD和ANWE的二阶校正方法得到的复杂背景下奥沙普秦的回收率令人满意,同时对本方法的精密度进行了研究。通过分析品质因子包括灵敏度(SEN)、选择性(SEL)、检出限(LOD)和检测量(LOQ),评估了这两种方法的性能,利用t-检验和椭圆置信区间(ECJR)统计方法对结果进行了校验。结果表明,解析准确可靠,方法快速简便,无需样品预处理,成本低廉,为临床及医药实时快速分析体液中奥沙普秦含量提供了新的定量分析方法。A new and effective approach was developed for the quantitative analysis of oxaprozin in human urine samples by the incorporation of excitation-emission matrix fluorescence（EEM） and second-order calibration methodologies based on self-weighted alternating trilinear decomposition（SWATLD） and alternating normalization-weighted error（ANWE） algorithms,respectively.With the application of a second-order advantage,excitation spectral profiles and emission spectral profiles of oxaprozin were effectively resoluted,even in the presence of urine and other homogeneous drugs such as nabumetone or naproxen.The average recoveries of oxaprozin in urine samples and the precision of test results are satisfactory.In addition,the accuracy of these two algorithms was also evaluated through figures of merit,such as sensitivity（SEN）,selectivity（SEL）,limit of detection（LOD） and limit of quanti-ication（LOQ）.Both methods were verified by t-test and the elliptical joint confidence region.The results show that both algorithms were accurate and reliable.The method is simple,without previous separation procedure.

关 键 词：奥沙普秦 三维荧光光谱 二阶校正 萘丁美酮 萘普生 自加权交替三线性分解 交替归一加权残差算法 

分 类 号：R96[医药卫生—药理学]