Determination of melatonin in commercial preparations by micellar electrokinetic chromatography and spectrofluorimetry

Melatonin was determined in pharmaceutical preparations by means of two simple and reliable analytical methods based on micellar electrokinetic chromatography (MEKC) and spectrofluorimetry. The fluorescence emission values were measured at λ=350 nm when exciting at λ=275 nm. The MEKC analysis was achieved using a system consisting of 40 mM SDS in phosphate buffer (20 mM, pH 7.5). The extraction of melatonin from the tablets was achieved by means of a simple one-step dissolution with methanol/water. Both methods were applied for the determination of melatonin in commercial formulations and galenic preparations. The MEKC procedure allows the quantitative determination of melatonin in all pharmaceutical preparations tested. On the contrary, the spectrofluorimetric method is not suitable for tablets which also contain tryptophan; this interference can be eliminated by a suitable liquid-liquid extraction procedure. The results obtained with the two methods are in good agreement and satisfactory in terms of precision and accuracy.     

同步荧光法同时测定苯甲酸和水杨酸的研究

根据苯甲酸与水杨酸在酸性条件下荧光光谱出现的差异，用同步荧光法同时测定其混合物中二组份。苯甲酸及水杨酸的检测限分别为０．２４μｇ／ｍＬ和０．２５μｇ／ｍＬ相对标准偏差分别为１．３％和１．２％。方法用于商品杀菌腐剂中苯甲酸与水杨酸的同时测定，结果满意。     

用同步荧光法研究细胞色素C在水溶液中的存在形态

用同步荧光光谱法研究细胞色素Ｃ在水溶液中的存在形态，发现细胞色素Ｃ中色氨酸残基的同步荧光光谱随浓度改变而发生变化，在较稀的溶液中，只观察到色氨酸残基的一个荧光峰，在较浓的溶液中也观察到一个荧光峰，而在这两个浓度之间时，这两个峰共存，可能反映了细胞色素Ｃ在不同浓度溶液中聚集状态的不同，当向存在两个荧光峰的溶液中加入不同浓度的脲，在一定脲浓度范围内，细胞色素Ｃ不发生变性，脲的作用使细胞色素Ｃ的单体浓度     

Spectrofluorimetric determination of human serum albumin using a doxycycline-europium probe

A new spectrofluorimetric method is proposed for determination of human serum albumin (HSA) with the limit of detection at ng levels. Using doxycycline (DC)-europium (Eu³⁺) as a fluorescent probe, in a buffer solution of pH 10.2, HSA can remarkably enhance the fluorescence intensity of the DC-Eu³⁺ complex at 612 nm and the enhanced fluorescence intensity of Eu³⁺ is proportional to the concentration of HSA. Optimum conditions for the determination of HSA are also investigated. The linear ranges for HSA are 0-9.2 and 9.2-34.5 μg ml⁻¹ with limits of detection of 64 and 115 ng ml⁻¹, respectively. This method is simple, practical and relatively free of interference from coexisting substances, as well as much more sensitive than most of the existing assays. The determination results for human serum and urine samples are identical to those by the AOAO method, with relative standard deviations of five determinations of 1.1-3.6%. By the Rosenthal graphic method, the binding number and association constant of human serum albumin with the probe are 1.8 and 3.71×10⁵ l mol⁻¹, respectively.     

1, 8-Dihydroxyanthraquinone-Ca(II) Reaction. Spectrofluorimetric Determination of Traces of Ca(II)

Abstract

1, 8-Dihydroxyanthraquinone (1, 8-DHAn) shows a fluorescent reaction with Ca(II) ion in ethanol-water mixtures and ammoniacal medium.

In the present work the 1, 8-DHAn-Ca(II) complex has been studied spectrofluorimetrically. The complex shows two excitation maxima at 485 nm and 495 nm and its emission maximum is centered at 615 nm. A 2:1 (R:C) stoichiometry and a log K_est of 7.38±0.22 for the overall equilibrium have been found for the complex.

A new method for the spectrofluorimetric determination of Ca(II) between 50 and 550 ngml^?1 has been proposed. The interference level of foreign ions has been established.     

Spectrophotometric and Spectrofluorimetric Determination of Famotidine and Ranitidine Using 1,4-Benzoquinone Reagent

ABSTRACT

Spectrophotometric and spectrofluorimetric methods were adopted for the analysis of Famotidine and Ranitidine depending on their reaction with 1,4 Benzoquinone reagent at pH 5.2 and 5.6, respectively. The absorbances of the resulting condensation products were measured at 502 and 508 nm for Famotidine and Ranitidine, respectively. Concentrations adhering to Beer's law were from 40-160 μg.ml^? for Famotidine and from 20-100 μg.ml^? for Ranitidine.

Furthermore the resulting condensation products exhibited fluorescence at 665 nm when excited at 290 nm and the calibration graphs were rectilinear from 0.4-1.4 μg.ml^? for Famotidine and from 0.21 μg.ml^? for Ranitidine.

Different parameters affecting these reactions were thoroughly studied. Also these methods were applied to the pharmaceutical preparations and the results were satisfactory. The validities of the methods were ascertained by the standard addition technique revealing fine results in consideration to the mean recovery percent and standard deviation.

The spectrofluorimetric method was a hundred times more sensitive then the spectrophotometric method. The proposed methods were sensitive, accurate, and precise as statistically compared with the official methods of analysis of Famotidine and Ranitidine.     

Determination of the Phytohormone Indole-3-Acetic Acid by Synchronous Derivative Spectrofluorometry Following Acetic Anhydride Derivatization

Abstract

The very selective fluorogenic reaction of indole-3-acetic acid (IAA) with acetic anhydride, acid catalyzed, is used to perform an improved fluorometric method for the determination of nanogram amounts of IAA. The synchronous derivative approach used in this work provides significant advantages in the more relevant analytical figures of merit, especially in sensitivity and precision.     

丙三醇存在下硫酸钡微粒体系的光谱特性研究及其分析应用

0.10 mol/L HCl-4.0 mol/L丙三醇-0.05 mol/L BaCl2溶液体系的瑞利散射很弱.当有SO4^2-存在时,（BaSO4）n微粒体系在470 nm处产生一较强的瑞利散射峰,SO4^2-浓度在1.0～80μg/mL浓度范围内与I470nm呈线性关系.据此,建立了一个测定水中硫酸根的简便、灵敏的瑞利散射光谱分析新方法.研究结果表明：SO4^2-与Ba^2＋由于静电引力可形成BaSO4分子,而BaSO4分子间存在较强疏水作用力和分子间作用力,可聚集形成（BaSO4）n微粒和固液界面,（BaSO4）n微粒和固液界面的形成是导致体系瑞利散射强的根本原因.     

同步荧光光谱分析中几个问题的探讨

通过实验阐明了同步荧光光谱与普通荧光光谱之间的关系，在此基础上讨论了溶剂散射光对同步荧光分析的影响以及同步荧光分析的灵敏度。     

化学计量学-同步荧光光谱法同时测定速灭威、残杀威和呋喃丹

在pH 4.0的B-R缓冲溶液中,速灭威、残杀威和呋喃丹能够产生内源荧光,但光谱严重重叠。当波长差Δλ=30 nm时,加入一定量的β-环糊精,3种农药的荧光强度均有不同程度的加强,且荧光强度与农药的浓度呈良好的线性关系,速灭威、残杀威和呋喃丹单组分的测量线性范围分别为0.2~2.0、0.02~0.38和0.04~0.56μg/mL;检出限分别为0.083、0.015和0.020μg/mL。应用多种化学计量学方法,如经典最小二乘(CLS)、主成分回归(PCR)和偏最小二乘(PLS)对同步荧光光谱严重重叠的3种农药混合体系合成样进行光谱解析并比较其分析能力。结果表明,PLS预报各组分的结果较好,采用该模型分析了一些实际食品样品,获得满意的结果。