苯基荧光酮荧光分光光度法测定痕量锗的研究

锗具有增血、抗炎症、抗衰老等多种医疗功能 ,因此 ,越来越受到人们的关注。荧光光度法测定微量锗已有报道[1～ 4] 。用苯基荧光酮荧光度法测定锗未见报道。本文利用苯基荧光酮与锗在醋酸 醋酸钠缓冲溶液中络合物形成速度快的优势 ,使其先在缓冲溶液中显色 ,然后在 0 .3ｍｏｌ ＬＨＣｌ介质中测定其荧光强度 ,用于粉煤灰中痕量锗的测定 ,得到满意结果。1　实验部分1 1　仪器与试剂ＲＦ - 5 4 0荧光分光光度计 (日本岛津 )。锗标准溶液 ( 1ｇ Ｌ) :称取 0 .1 0 0 0ｇ纯锗粉于 5 0ｍｌ小烧杯中 ,加入 5ｍｌＮａＯＨ ,再加入几滴 30 %Ｈ2 Ｏ2…     

Determination Of V(V) By Means Of 1-Amino-4-Hydroxynthraquince By A Kinetic Spectrofluorimetric Method

Abstract

A kinetic method of spectrofluorimetric determination of V(V) is established based on the reaction of the cation with 1-amino-4-hydroxyanthraauinone, in which formation of an oxidation product of the reagent takes place. The variables that influence the development of the fluorescence are studied and the influence that the presence of foreign ions may cause is determined, finding that only Ce(lV) interferes seriously when it is in concentrations higher than that of V(V). The method is applied to the determination of non volatile vanadium in petroleum crudes.     

Combination of ionic liquid-based dispersive liquid-liquid micro-extraction with stopped-flow spectrofluorometry for the pre-concentration and determination of aluminum in natural waters, fruit juice and food samples

In this research, we combined ionic liquid-based dispersive liquid-liquid micro-extraction (IL-based DLLME) with stopped-flow spectrofluorometry (SFS) to evaluate the concentration of aluminum in different real samples at trace level. 1-Hexylpyridinium hexafluorophosphate [Hpy][PF₆] ionic liquid and 8-hydroxyquinoline (oxine), which forms a highly fluorescent complex with Al³⁺, were chosen as the extraction solvent and chelating agent, respectively. The hydrophobic Al-oxine complex was extracted into the [Hpy][PF₆] and separated from the aqueous phase. Then, the concentration of the enriched aluminum in the sediment phase was determined by SFS. Some effective parameters that influence the SFS signals and the micro-extraction efficiency, such as the suction and sending time, the concentration of the chelating agent, pH, the amount of the ionic liquid, the type of disperser solvent and diluting agent, ionic strength, extraction time, equilibration temperature and centrifugation time were investigated and optimized. In the optimum experimental conditions, the limit of detection (3 s) and enrichment factor were 0.05 μg L⁻¹ and 100, respectively. The relative standard deviation (RSD) for six replicate determinations of 6 μg L⁻¹ Al was 1.7%. The calibration graph using the pre-concentration system was linear in the range of 0.06-15 μg L⁻¹ with a correlation coefficient of 0.9989. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of aluminum in several water, fruit juice and food samples.     

Liquid phase microextraction applications in food analysis

Over the last years, liquid-phase microextraction (LPME) in its different application modes (single drop microextraction, dispersive liquid-liquid microextraction and hollow fiber-LPME) has been increasingly applied for the extraction of both inorganic and organic analytes from different matrices. Its advantages over conventional extraction procedures (simplicity, effectiveness, rapidity and low consumption of organic solvents) has also attracted its application in the complex food analysis field, in which it has clearly provided good and challenging results. A comprehensive review dealing with those articles published since its introduction till the end of March 2011 is presented, offering also a critical vision of the analytical potential of LPME for the analysis of foods.     

停流-抑制动力学荧光法测定痕量苯酚

用停流技术研究了在H2SO4介质中,苯酚抑制BrO-3氧化丁基罗丹明B荧光猝灭反应,并探讨了反应机理。基于苯酚对该反应诱导期的影响作用,建立了停流-抑制动力学荧光法测定痕量苯酚的新方法。方法的检出限为1.4×10-8g.L-1,线性范围为0.4~15.0μg.L-1,11次测定7.0μg.L-1苯酚的相对标准偏差为2.1%。本法灵敏、简便,用于测定制药废水和番茄酱样品中痕量苯酚,结果满意。     

Spectral inhomogeneity and wavelength-dependent rotation of probe molecules in membranes

Using subnanosecond laser spectrofluorometry, the spectral and polarization time-resolved characteristics of 1-phenylnaphthylamine (1-AN) fluorescent probe in phospholipid bilayer and red blood cell (RBC) membranes have been studied. It is shown that the electronic spectra of the probe in model-membranes are inhomogeneously broadened. In contrast to low-molecular weight solvents, there are two reasons for inhomogeneous broadening. The first is connected with different levels of location of probe molecules in the membrane. Inhomogeneous broadening due to the first factor has a static character. The second reason is similar to that of solutions and linked with fluctuations of solvate structure. This type of broadening has a dynamic character. The process of intermolecular relaxation in membranes is accompanied by the release of the free energy excess, which results in wavelength-dependent rotation of probe.     

Spectrofluorometric determination of mercury (II) with murexide

A very sensitive and selective spectrofluorometric method has been developed for Hg(II) determination in pharmaceutical and environmental samples. The method is based on measuring the decrease in fluorescence intensity of murexide after binding Hg(II) . The intensity of the fluorescence emission peak was measured at ex/em 335/435 nm in several buffer solutions (acetic acid/acetate, NaH₂PO₄/Na₂HPO₄, NH₄ ⁺/NH₃) targeting the pH interval 3.0–9.0. The fluorescence intensity decrease was found to be linear in the concentration range of 8 × 10^–7 to 1 × 10^–5 M of Hg(II) by using 5 × 10^–5 M murexide in 0.1 M acetic acid/acetate buffer at pH 4.2. The detection limit was 2 × 10^–7 M. This method was found to be almost free of interference from large excesses of 40 cations and anions. The method was successfully applied to the analysis of Hg(II) in synthetic mixtures, pharmaceutical preparations, and wastewater samples. The recovery was quantitative and the standard deviation for 10 replicates of a sample containing 1 × 10^–6 M Hg(II) was lower than ±4%.     

Study on the Supramolecular Interactions of p-Sulfonated Calix[4, 6, 8]arenes with Lomefloxacin

The supramolecular interactions between a homologous series of p-sulfonated calix[n]arenes (SCnA, n = 4, 6, 8) as hosts and lomefloxacin (LFLX) were studied by spectrofluorometry. LFLX was found to react with SCnA to produce stable complexes. The fluorescence intensity of the complexes decreased gradually with increasing SCnA concentration. The formation of complexes was further confirmed by ¹H NMR studies and molecular modeling calculations. Data of the stability constants and thermodynamic parameters of the obtained complex showed that the stability of the SC8A-LFLX complex is superior to that of SC6A-LFLX and SC4A-LFLX. A mechanism was proposed to explain the inclusion process.     

Vortex-Assisted Acid-Induced Cloud Point Extraction Coupled With Spectrofluorometry for the Determination of Fluoroquinolones in Environmental Water Samples

The present work describes a simple and rapid extraction approach based on vortex-assisted acid-induced anionic surfactant sodium dodecyl sulfate-mediated extraction (vortex-assisted acid-induced cloud point extraction) prior to spectrofluorometry for the determination of four fluoroquinolones, including norfloxacin, ciprofloxacin, sarafloxacin, and gatifloxacin, in water samples (hospital wastewater, river water, lake water, and water from the inlet of a wastewater treatment plant). Sodium dodecyl sulfate and concentrated hydrochloric acid (12 mol/L) were used as extractants. The four fluoroquinolones were concentrated in the surfactant-rich phase after phase separation and were determined by a spectrofluorophotometer. Some parameters affecting the extraction efficiency, such as the type and amount of surfactant, the amount of acid, vortex treatment, and centrifugation, were optimized systematically. Under the optimized conditions, the proposed method showed good analytical features with linearity for all analytes in a wide range of 0.045–0.90 µg/mL and coefficients of determination no less than 0.9901. The limits of detection (S/N = 3) were 0.007, 0.010, 0.009, and 0.013 µg/mL for norfloxacin, ciprofloxacin, sarafloxacin, and gatifloxacin, respectively; good precisions expressed as the relative standard deviations were in the range of 0.9–3.7% (n = 6); and average recoveries at three spiking levels ranged from 83.0% to 96.7%. The results of the proposed method are comparable to those obtained from the high-performance liquid chromatography method (t-test, p = 0.05) and are reliable for determination of fluoroquinolones in environmental water samples.     

A Kinetic Fluorimetric Method for Determination of Microamounts of Pt(IV) with 2-2′ Dipyridylketone Hydrazone

Abstract

A kinetic method for determination of traces of Pt(IV) based on the aerobic oxidation of the hydrazone of 2-2′ dipyridylketone, in which the formation of a fluorescent product (λ_ex = 359 nm, λ_em = 435 nm) takes place, is described. The reaction is followed by the measurement of the rate of appearance of the fluorescence. The proposed method suffers very few interferences.