主成分回归-紫外光度法同时测定食用香料麦芽酚和乙基麦芽酚

报道了一种快速、简便的同时测定食用香料麦芽酚、乙基麦芽酚光度法,方法基于在pH2.87的B R缓冲溶液中对麦芽酚和乙基麦芽酚两组分混合溶液进行光度测定,所得的重叠波谱数据用主成分回归法(PCR)、经典最小二乘法(CLS)和偏最小二乘法(PLS)等化学计量学方法进行处理,结果表明主成分回归法(PCR)的预报误差最小。对样品进行测定,获得了较好的定量分析结果。麦芽酚和乙基麦芽酚的线性范围均为1.0～20.0mg·L-1;检出限分别为0.4347和0 5589mg·L-1。     

主成分回归一紫外光度法同时测定盐酸西替利嗪和苯甲酸钠

提出了一种用紫外光度法同时测定盐酸西替利嗪和苯甲酸钠的方法.在pH 4.56的B-R缓冲溶液中对盐酸西替利嗪和苯甲酸钠两组分混合溶液进行吸光度测定,所得的重叠光谱数据用主成分回归法(PCR)和偏最小二乘法(PLS)等化学计量学方法进行处理,结果表明主成分回归(PCR)的预报误差最小.对实际样品进行测定,回收率为88.8...     

UV–Second Derivative Spectrophotometric and Colorimetric Methods for the Determination,Validation and Thermogravimetric Analysis of New Oral Antidiabetic Pioglitazone in Pure and Pharmaceutical Preparations

Abstract

Three rapid, sensitive, and simple spectrophotometric methods have been developed for the determination of pioglitazone in pure and pharmaceutical preparations.

For the first method, UV-spectrophotometry, standard solutions were measured at 270.2 nm. The first method was linear from 5.0–20.0 µgmL^?1. The linearity was found to be 5.0–20.0 µgmL^?1. For the second method, the distances between two extremum values (peak-to-peak amplitudes), 272.0 and 287.4 nm were measured in the second order derivative-spectra of standard solutions. Calibration curves were constructed by plotting d² A/dλ² values against concentrations, 2.0–12.0 µgmL^?1 of pioglitazone standards in acetonitrile. The detection limits of pioglitazone were 0.10 and 0.16 µgmL^?1 for UV and derivative spectrophotometric methods, respectively. The third method was based on the formation of an ion association complex with bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB), and bromothymol blue (BTB). The assay was linear over the concentration range of 20.0–100.0 µgmL^?1 for BCG, 10.0–100.0 µgmL^?1 for BCP, 20.0–120.0 µgmL^?1 for BPB, and 10.0–100.0 µgmL^?1 for BTB. The detection limits of pioglitazone was found to be 0.14 µg mL^?1 for BCG, 0.32 for BCP, 1.24 µgmL^?1 for BPB, and 0.22 µgmL^?1 for BTB. The thermal analysis of the pioglitazone was studied by Thermogravimetric Analysis-Differential Scanning Calorimetry (TGA-DSC) techniques. Enthalpy change of pioglitazone was found to be 85.16 J/g. The proposed methods were validated according to the ICH guidelines (1996) with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness. The results demonstrated that the procedure is accurate, precise, specific, and reproducible (percent relative standard deviation <2%), while being simple and less time consuming. The three proposed methods have been successfully applied to the assay of pioglitazone in pure and in pharmaceutical preparations. The results compared with those obtained by an ultraviolet spectrophotometric method using t and F tests.     

化学计量学辅助紫外分光光度法同时测定洛美沙星和司帕沙星

在pH：3．0的B-R缓冲溶液中,洛美沙星（LMX）和司帕沙星（SPFX）的最大吸收波长分别为286nm和296nm,两者吸收光谱严重重叠．本文用多元线性回归（MLR）、K-矩阵（AKC）、P-矩阵（CPA）等计算方法辅助紫外分光光度法,同时测定了模拟样中LMX和SPFX的含量。发现CPA法明显优于MLR和AKC,LMX和SPFX的平均回收率分别达99．5％和99．9％,相对标准偏差RSD分别为0．59％和0．85％.     

酸性介质中品红与亚硝酸根的显色反应研究

根据酸性介质中品红与亚硝酸根反应的现象及光谱特征，采用连续变化法确定生成物的组成、结构，提出了重氮化反应原理，解释了红移等现象。     

多波长线性回归紫外吸光光度法同时测定炼油厂污水中苯酚和苯胺

提出用多波长线性回归紫外吸光光度法同时测定炼油厂污水中的苯酚和苯胺.方法省去了萃取、蒸馏、显色等步骤,操作简单.对合成水样进行测定,相对标准偏差≤4.57%,相对误差≤±2.3%.对炼油厂水样进行测定并进行加标回收试验,苯酚和苯胶的回收率分别为99.4%～103.0%和97.2%～104.0%,结果良好.苯酚和苯胶的最低检出限分别为0.010和0.048μg·ml~(-1).     

紫外吸光光度法同时测定乙醛酸和乙二醛

利用醛基与羟胺在酸性条件下的加成反应产物乙醛酸肟和乙二醛二肟的不同紫外吸收峰,用双波长法同时测定溶液中的乙醛酸和乙二醛。结果表明,乙醛酸在 0.03~0.156 g·L-1范围内符合比耳定律,其回归方程为 y=0.109 4x-0.003 7,r=0.999 9(n=5),乙二醛在 0.1~0.5 g·L-1范围内符合比耳定律,其回归方程为y=0.223 11x-0.023 5,r=1.000 0(n=5)。乙醛酸和乙二醛质量比大于1,乙醛酸的回收率为 96.2%~101.5%,乙二醛的回收率为 101.6%~106 8%。方法操作简便、经济、精密度较好。     

Spectroscopic Study of Some Alkali and Alkaline Earth Complexes with Benzo Crown Ethers in Ethanol Solution

The interaction between Na⁺, K⁺, Mg²⁺ and Ca²⁺ ions and benzo crown ethers B15C5, DB18C6, DB21C7, DB24C8 and DB30C10 in ethanol solution has been studied spectrophotometrically at 25°C. The formation constants for 1:1 complexes were determined by computer fitting of the resulting UV-absorbance-mole ratio data. In the case of all crown ethers used, K⁺ ion was found to form the most stable complexes. The observed selectivities of different benzo crowns for the cations used are discussed in terms of the cavity-cation size ratio, number of the donating oxygens participating in the cation binding, conformations of the free and complexed ligands and ionic solvation.     

人工神经网络用于紫外光谱同时测定苯和甲苯及二甲苯的含量

根据反向传输（Backpropagation,BP）算法,应用三层ANN（人工神经网络,Artificial neural network）网络原理,对紫外光谱严重重叠的苯、甲苯和二甲苯的混合体系进行同时测定。在230～280nm范围内,以16个特征波长处的紫外吸光度作为网络特征参数,并通过均匀设计安排样本进行网络训练和计算。苯、甲苯和二甲苯的回收率依次为98．7％,99．4％和97．4％,测定结果的相对标准偏差分别为2．0％,2．8％和2．7％。     

一阶导数紫外分光光度法测定2,6-二硝基氯苯-4-磺酸

选用248 nm作为一阶导数紫外分光光度法测定2,6-二硝基氯苯-4-磺酸的测定波长可避免一些共存杂质的干扰,在选定的最佳条件下,被测化合物浓度在0~81.24 mg.L-1之间与其一阶导数值呈线性关系,相关系数为0.999 8,测得方法的检出限(3σ/s)为2.39 mg.L-1。从3个不同批号的产物中取样分析,测得结果的平均相对标准偏差(n=6)为0.17%,进行了标准加入法回收率试验,所得结果在99.5%~100.1%之间。