分辨荧光光谱严重重叠药物体系的惩罚对角化误差算法

水杨酸、龙胆酸和对-氨基苯甲酸是3种荧光光谱严重重叠的常用药物，用常规方法难以同时测定；运用新近提出的惩罚对角化误差算法(the algorithm with the penalty diagonalization error,PDE)结合三维荧光分析法，对该体系进行了研究，研究结果表明该算法不仅能用于荧光光谱严重重叠体系的分辨，而且具有收敛速度快及对组分数估计不敏感性的优点。     

三维荧光光谱总体积积分法同时测定维生素B2和B6

运用三维荧光光谱总体积积分法建立了一种测定维生素Ｂ２和Ｂ６的荧光分析新方法，该方法的度较常规峰值法分别提高１３０和３１０倍，同时成功地应用于两者的同时测定。     

多元分辨校正模型与方法研究—无机多组份分析

系统研究了各种多元分辨校正模型、方法及其应用，以模拟体系、病态体系有态体系为对象，考察了它们的多元校正能力与多元分辨效果，给我机多组份分析态体系实例。     

多元校正分光光度法同时测定兔血清内的氨甲苯酸和酚磺乙胺

氨甲苯酸和酚磺乙胺在紫外区均有吸收,但吸收光谱重叠而形成干扰,较难直接进行分析。本文采用紫外分光光度法对氨甲苯酸和酚磺乙胺两组分混合溶液进行测定,并将所得光谱数据用化学计量学多元校正方法处理。本法测定氨甲苯酸和酚磺乙胺的的线性范围均为2.0~20.0μg/mL。用拟定的方法测定了兔血清中的氨甲苯酸和酚磺乙胺,并与高效液相色谱法的结果进行了比较,两者无显著性差异。     

Simultaneous Determination of Dextromethorphan and Quinidine Contents in Biological Fluid Samples Using Excitation-Emission Matrix Fluorescence Coupled with Second-Order Calibration Methods

This paper presents a novel method for simultaneous determination of dextromethorphan and quinidine contents in biological fluid samples using excitation–emission matrix fluorescence (EEM) coupled with second-order calibration methods. The adopted calibration methods, i.e., parallel factor analysis (PARAFAC), self-weighted alternating tri-linear decomposition (SWATLD), and alternating penalty trilinear decomposition (APTLD), could adequately exploit the second-order advantage. The accuracy of the three methods was evaluated through figures of merit and elliptical joint confidence region (EJCR) tests. It has been found that all the methods could give good results. But, with correct number of factors, the PARAFAC model performed slightly better than the others.     

Simultaneous Polarographic Determination of Lead (II) and TIN (II) by Multivariate Calibration

ABSTRACT

The polarographic waves of lead (II) and tin (II) overlap due to their similar reductive potentials and it is difficult to determine these two components simultaneously without a pre-separation. In this paper, differential pulse polarography (DPP) combined with multivariate calibration approaches, such as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS), were successfully applied to the resolution of overlapping polarographic waves of these two components in the concentration range of 0.05-3.50 mg 1^?1. Satisfactory quantitative results were obtained.     

三维荧光二阶校正同时测定人体液中伊立替康及其代谢物7-乙基-10-羟基喜树碱的含量

提出了激发发射矩阵荧光光谱与化学计量学二阶校正方法相结合用于同时快速定量人体液(血浆和尿液)中的伊立替康(CPT11)和其主要代谢产物7-乙基-10-羟基喜树碱(SN38)的绿色、高灵敏分析策略. 尽管其分析物之间以及分析物和背景之间的光谱存在严重重叠现象, 采用基于交替归一加权残差(ANWE)算法的二阶校正方法进行解析仍能得到令人满意的定性定量分析结果. 当该体系的组分数选取为3时, 可以得到血浆和尿液中CPT11的平均回收率分别为(96.8±6.3)%和(101.7±1.1)%, SN38在血浆和尿液中的平均回收率分别为(100.4±4.9)%和(101.6±1.1)%. 另外, 通过品质因子, 如灵敏度(SEN)、选择性(SEL)、检测下限(LOD)和定量检测限(LOQ)评估了该方法的准确性. 实验结果表明, 该方法能以“数学分离”代替繁琐的“物理和化学分离”, 成功地解决实际复杂体系中内源干扰物质与分析物光谱重叠所引起的难分辨的问题, 可用于人体液中CPT11和SN38含量的直接快速定量测定.     

三维荧光光谱总体积积分法同时测定多环芳烃

提出了三维荧光光谱总体积积分法并应用于多环芳烃萘、芘、Ｂｅｉ的同时测定，结果表明，三维荧光光谱总体积积分法不仅可以同时测定萘、芘、Ｂｅｉ而且灵敏度（信噪经）常规法分别提高２２、３３和２６倍同时并考察了积分区域对灵敏度的影响。     

Rapid Resolution RP-HPLC-DAD Method for Simultaneous Determination of Sildenafil,Vardenafil, and Tadalafil in Pharmaceutical Preparations and Counterfeit Drugs

A novel and Rapid Resolution Reversed-Phase High-Performance Liquid Chromatography-Diode Array Detector method has been developed and validated for the simultaneous determination of sildenafil, vardenafil, and tadalafil in pharmaceutical preparations and counterfeit drugs. An Agilent Zorbax SB C8 column (50 × 4.6 mm i.d., 1.8 μm particle size) was used. The mobile phase consisted of a mixture of 0.030 M of ammonium formate (adjusted to pH 3.0 with formic acid) and acetonitrile in the ratio 70:30. Ultraviolet (UV) detection was performed at 230 nm. Total run time was 7 min; these three drugs were eluted at the retention times of 1.654, 2.032, and 5.067 min for vardenafil, sildenafil, and tadalafil, respectively. The method was validated for accuracy, precision, linearity, specificity, and sensitivity. From the validation study, it was found that the method is specific, rapid, accurate, precise, and reproducible. Calibration curves were linear over the concentration ranges of 0.2–200 μg ml^?1 for sildenafil, vardenafil, and tadalafil. The limits of detection (LOD) values were 1.0, 1.1, and 1.0 ng and the limit of quantification (LOQ) values were 2.0, 2.1, and 2.0 ng for sildenafil, vardenafil, and tadalafil, respectively. The method is rapid both for routine quantitative analysis of sildenafil, vardenafil, and tadalafil in pharmaceutical preparations and screening their suspected counterfeit drugs.     

三维荧光二阶校正法用于血浆和尿液中柔红霉素的快速测定

文章采用三维激发发射荧光光谱与化学计量学交替三线性分解(ATLD)二阶校正法相结合,对血浆液和尿液中柔红霉素(DM)进行定量测定。实验不需对血浆和尿液预测样进行萃取等分离预处理,选取激发波长410～530nm,发射波长550～650nm,分别每隔5nm取一个数据,利用激发发射荧光扫描分别获得两个三维响应数阵(大小为21×25×12)。当组分数选择为3时,血浆和尿液校正集中盐酸柔红霉素的相对浓度与实际浓度的相关系数分别为r1=0.9990和r2=0.9952,经ATLD算法解析得到的血浆和尿液预测样中柔红霉素平均回收率分别为(92.8±7.6)%和(94.7±4.4)%。实验结果表明,此法能够解决血浆和尿液中盐酸柔红霉素药物因血浆和尿液内源物质与分析物光谱重叠所引起的难分辨的问题,可用于未知干扰共存下柔红霉素的直接快速定量测定。