Fluorimetric Determination of Histamine in Fish Using Micellar Media and Fluorescamine as Labelling Reagent

An analytical method based on the use of fluorescamine to produce a fluorescent derivative with histamine and combined with micellar-enhanced fluorescence detection of the formed complex is developed for the sensitive and rapid determination of histamine in fishes. The fluorescence properties of the obtained complex in water and micellar solutions of sodium dodecyl sulfate (SDS), cetyltrimethylammonium chloride (CTAC) and brij-700 are reported. Physicochemical variables influencing the sensitivity of the method (pH, micellar, fluorescamine and NaCl relative concentrations) have been optimized. The stability of the formed complex, as shown by kinetic study, depends on the pH of the solution. Linear calibration curves allowing an effective histamine determination were established with large linear dynamic range (LDR), and low limits of detection (LOD) between 0.5 and 33 ng mL⁻¹, according to the solvent. Application to the analysis of fish samples (sardines) yielded satisfactory results. The method seems to be suitable for environmental fish quality control. Presented in part, at the 39th IUPAC Congress and the 86th Conference of the Canadian Society for Chemistry, August, 10–15, 2003, Ottawa (Canada).     

Structural Changes in Human Serum Albumin According to the Data on the Phosphorescence Kinetics of a Luminescent Probe — Eosin

The influence of the human serum albumin (HSA) denaturation by a surface-active substance (sodium dodecyl sulfate (SDS)) on the phosphorescence of a luminescent probe (eosin) has been investigated. The dependences of the eosin-phosphorescence intensity on the SDS concentration were determined at different pH levels of an HSA solution. It has been shown that at SDS concentrations lower than the critical concentration necessary for micelle formation, the hydrophobic interactions of eosin with the protein influence the deactivation of the eosin triplet states. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 72, No. 5, pp. 660–663, September–October, 2005.     

Facile synthesis,growth mechanism,and optical properties of CdSe nanoparticles in self-assembled micellar media and their efficient conjugation with proteins

This article demonstrates the influence of various surfactants of different polarities—anionic, sodium dodecyl sulfate, cationic, hexadecyltrimethylammonium bromide and non-ionic, and polyoxyethylene iso-octyl phenyl ether (TX-100)—on the formation of CdSe nanoparticles in aqueous solutions. The surfactant-stabilizing effect has been monitored using transmission electron microscopy. Spectral properties of CdSe nanoparticles have been investigated; the structure of the long-wave edge of the fundamental absorption band of CdSe nanoparticles has been analyzed. It has been shown that the variation of the synthesizing conditions (stabilizer’s nature and concentration, CdSe concentration, etc.) allows the tailoring of the CdSe nanoparticle size in the range of 8–17 nm. Lifshitz–Slyrzov–Wagner kinetic analysis has also been performed using the size variation according to ripening temperature and time period. The differences in the stabilization ability of tested substances are discussed with respect to their structure and possible mechanism of the surface interaction with the nanoparticles. The flexible surface chemistry of the CdSe-micelles causes them to be water soluble and allows their further conjugation with protein molecules through electrostatic attraction. The interaction between functionalized CdSe nanoparticles with protein molecules have been investigated using fluorescence spectroscopy.     

Micelle-Enhanced Spectrofluorimetric Method for Determination of Cholesterol-Reducing Drug Ezetimibe in Dosage Forms

A simple and sensitive spectrofluorimetric method was developed for the determination of ezetimibe in its pharmaceutical formulations. The proposed method is based on investigation of the fluorescence spectral behavior of ezetimibe in sodium dodecyl sulfate (SDS) micellar system. In aqueous solution of acetate buffer pH 5.0, the fluorescence intensity of ezetimibe was greatly enhanced, 200% enhancement, in the presence of SDS. The fluorescence intensity of ezetimibe was measured at 380 nm after excitation at 268 nm. The fluorescence-concentration plot was rectilinear over the range of 0.03–3.0 μg/mL with lower detection limit of 3.08 × 10⁻³ μg/mL. The method was successfully applied to the analysis of ezetimibe in its commercial tablets; the results were in good agreement with those obtained with the reported method. The application of the proposed method was extended to the stability studies of ezetimibe after exposure to different forced degradation conditions, such as acidic, alkaline, photo and oxidative conditions, according to ICH guidelines.     

Optical properties of silicon-silicide nanoheterostructures grown by consecutive plasma-epitaxy synthesis

Consecutive plasma-epitaxial synthesis on silicon wafers is used for the first time to fabricate monolithic nanoheterostructures with embedded nanocrystals (NC) of chromium disilicide (Si–NC CrSi₂–Si). It is found that, initially, nanoislands form on the surface and within a coating layer of silicon, followed by the formation of small (10–15 nm) nanocrystals of semiconducting chromium disilicide (CrSi₂) at a high occupation density ((2–3)⋅10¹¹ cm^–2). During formation of silicon-silicide-silicon heterostructures, CrSi₂ nanocrystallites “float up” into the near surface area of the covering silicon layer.     

Regularities of triplet-triplet annihilation of aromatic hydrocarbons in aqueous micellar solutions of sodium dodecyl sulfate

Investigation of deactivation processes in triplet states of a series of aromatic hydrocarbon molecules (antracene, 1,2-benzantracene, and 3,4-benzpyrene) made it possible to reveal the presence of triplet-triplet annihilation of the molecules in aqueous micellar solutions of sodium dodecyl sulfate. It is shown that the effect of microheterogeneous solutions on the process of triplet-triplet annihilation manifests itself in an increase in the probability of excimerization upon dissociation of triplet pairs of 1,2-benzantracene and 3,4-benpyrene molecules compared to one-component solutions. Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 64, No. 5, pp. 626–628, September–October, 1997.     

The kinetics of solvolysis of phosphorus acid esters in the ternary sodium dodecyl sulfate-ethylene glycol -La3+ micellar system

By methods of conductivity measurements, micellization of sodium dodecyl sulfate in ethylene glycol at the concentration above 0.18 M is shown. The La³⁺ ion catalysis of solvolysis of phosphorus acid ester both in the absence of surfactant and in the micellar sodium dodecyl sulfate solution in ethylene glycol is found. The influence of the other lanthanide ions on the kinetics is also studied. The La³⁺ and Pr³⁺ are found to exert an identical effect while Sm³⁺ is less effective. By methods of polarizing microscopy, the formation of liquid crystalline mesophase at high lanthanum (tris(dodecyl)sulfate concentrations in ethylene glycol is revealed. The investigation of the catalytic effect of the sodium dodecyl sulfate -La³⁺ (3 : 1 molar) composition has shown a sharp acceleration of the reaction at high surfactant concentration.     

Resonance Rayleigh Scattering,Second-Order Scattering and Frequency Doubling Scattering Spectra of Copper(II)-Flutamide System with Anionic Surfactants and its Analytical Application

A simple, sensitive, and rapid method based on ion association, for the determination of FLD has been developed. Flutamide (FLD) can react with Cu(II) to form 1:1 cationic chelate at pH 2.2–7.0 Mclivaine buffer medium, which can further react with anionic surfactants (AS) such as sodium dodecyl sulfate (SDS), sodium lauryl sulfonate (SLS) and sodium dodecylbenzene sulfonate (SDBS) to form 1:1 ion-association complexes. As a result, the resonance Rayleigh scattering (RRS), second-order scattering (SOS) and frequency doubling scattering (FDS) were enhanced to the highest degree. The maximum RRS, SOS and FDS wavelengths of three ion-association complexes were located at 345/345 nm, 610/305 nm and 430/860 nm, respectively. The increments of scattering intensity (ΔI) were directly proportional to the concentration of FLD in certain ranges. The detection limits (3σ) of FLD for SDS, SLS and SDBS systems were 1.9 ng ml⁻¹, 2.1 ng ml⁻¹ and 2.2 ng ml⁻¹(RRS method), 2.4 ng ml⁻¹, 2.7 ng ml⁻¹ and 2.6 ng ml⁻¹ (SOS method) and 2.3 ng ml⁻¹, 2.4 ng ml⁻¹ and 2.5 ng ml⁻¹ (FDS method), separately. The sensitivity of RRS method was higher than those of FDS and SOS methods. The optimum conditions of RRS method and the influence factors, the composition and the reaction mechanism have been discussed. Since the method is highly selective, it does not interference concomitant substances. These methods were applied successfully for the determination of FLD in pharmaceutical formulation and urine samples.     

Silver nanoparticles as matrix for laser desorption/ionization mass spectrometry of peptides

Silver nanoparticle synthesized from chemical reduction has been successfully utilized as a matrix in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of peptides. Acting as a substrate to adsorb analytes, as well as a transmission medium for UV laser, silver nanoparticle was found to assist in the desorption/ionization of peptides with little or no induced fragmentation. The size of the nanoparticle was typically in the range of 160 ± 20 nm. One of the key advantages of silver nanoparticle for peptides analysis is its simple step for on-probe sample preparation. In addition, it also minimizes the interferences of sodium dodecyl sulfate (SDS) surfactant background signal, resulting in cleaner mass spectra and more sensitive signal, when compared to α–cyano-4-hydroxycinnamic acid (CCA) matrix.     

New fluorimetric reagents, sodium pyrophosphate, sodium trimetaphosphate, and sodium tetrametaphosphate, for the determination of cerium(III)

Three sensitive and selective new alternatives for fluorometric determination of cerium(III) are described in this study. Ce(III) is highly fluorescent in sodium pyrophosphate, sodium trimetaphosphate, and sodium tetrametaphosphate solutions. For these reagents, the maximum excitation/emission wavelengths are 300/350, 297/340, and 299/352 nm, respectively. Maximum fluorescence intensities are obtained by irradiating Ce(III) dissolved in 0.033 g L⁻¹ sodium pyrophosphate, 41.4 g L⁻¹ sodium trimetaphosphate, and 0.96 g L⁻¹ sodium tetrametaphosphate at room temperature. The fluorescence intensities are linear over the range 0.001–30, 0.001–75, and 0.001–70 μg ml⁻¹. The detection limits are calculated as 9.5 × 10⁻³, 1.1/10⁻³, and 3.8 × 10^-3 μg ml⁻¹ Ce(III), respectively. The relative standard deviations for 15/0.05 Μg ml⁻¹ Ce(III) are 1.1/1.2, 1/1.1, and 1.2/1.3%, respectively. Quenching effects of other lanthanides and some inorganic anions were investigated. The methods have been applied to rare earth mixtures with a good accuracy.     

Trace Measurement of Phenothiazine Drugs in Tablets by Micellar-Enhanced Fluorophotometric Method

It was found that in buffer solution of pH 7.0, the addition of sodium dodecyl sulfate (SDS) to the solution of phenothiazine drugs, such as chlorpromazine, promethazine and trifluoperazine, showed a remarkable enhancement of their fluorescence intensity. A further study proved that the phenothiazine drugs can be determined by fluorophotometric method in micellar system. Under optimal conditions, there was a good linear relationship between fluorescence intensity and phenothiazine compounds concentration, and the detection limit of 3.0×10^-8 M chlorpromazine, 3.0×10⁻⁸ M promethazine and 1.5×10⁻⁸ M trifluoperazine (S/N=3) were also obtained. This method has been used to determine phenothiazine drugs in tablets with satisfactory results.     

Phosphorescence properties of sol–gel derived ruby measured as functions of temperature and Cr<Superscript>3+</Superscript> content

A novel approach for the contactless measurement of surface temperatures is to evaluate the temperature dependent phosphorescence properties of chromium doped aluminium oxide (ruby) coatings, such as phosphorescence intensity, spectral distribution, or the phosphorescence lifetime. However, these properties are also affected by the chromium content in the films. In the present study the phosphorescence lifetimes were studied for the first time as a function of the chromium content. We use a simple sol–gel depositing technique for the preparation of precisely doped ruby coatings in Si(100) substrates. These coatings (Cr-to-Al-ratios y between 0% and 6.8 at. %) are well suited for studying the influence of the chromium concentration on the phosphorescence properties: at room temperature (294 K), the phosphorescence intensity is strongly affected by the chromium doping (maximum at y∼1–1.5%) while the spectrum shifts only slightly with varying chromium content. The phosphorescence lifetime τ at 294 K remains constant with varying Cr³⁺ content below y∼1.1%, and decreases strongly above y∼1.1%. Thus, ruby doped with y∼1% seems to be most promising as a temperature sensor because it shows the highest phosphorescence intensity and a low variance in the phosphorescence lifetimes. Due to the latter property the temperature evaluation from τ is less affected by imprecise doping. The phosphorescence lifetimes of several sol–gel ruby coatings (y=1.1%) on Si(100) substrates were measured as a function of the temperature to be between 2.7 ms at 294 K and 4 μs at 833 K. PACS 07.20.Dt; 78.55.-m; 78.66.-w     

Investigation on the Micelle-Sensitized Ce (IV) - Lornoxicam-Rh B Chemiluminescence System and its Application

Based on the micelle synergism mechanism, a simple and sensitive flow injection chemiluminescence (FI-CL) method for the assay of lornoxicam was described. The CL signal generated from the reaction of Ce (IV) with lornoxicam in acidic solution was very weak, while the interfusion of sodium dodecyl benzene sulfonate (SDBS) resulted in a highly CL intensity. Under the optimum experimental conditions, the CL intensity was proportional to lornoxicam concentration over the range 1.0 × 10⁻¹⁰–7.3 × 10⁻⁸ g/mL with a detection limit of 4.9 × 10⁻¹¹ g/mL (3σ). The relative standard deviation for 11 replicate measurements of 3.0 × 10⁻⁹ g/mL of lornoxicam was 1.9%. The proposed method was successfully applied for the assay of lornoxicam in pharmaceuticals, human serum and urine with excellent recovery. The possible mechanism of CL reaction was also discussed briefly.     

Luminescent spectral characteristics of eosin in solutions of human serum albumin when denatured by treatment with sodium dodecyl sulfate

From analysis of the fluorescence spectra of eosin molecules in a solution with human serum albumin (HSA), we have obtained information about the dynamics of protein conformational rearrangements during denaturing of the protein when treated with sodium dodecyl sulfate (SDS) for different pH values of the solution. We hypothesize that HSA denaturing in the presence of SDS occurs in two stages: the first stage is loosening of the protein globules, and the second stage is complete unfolding of the protein molecules. We have shown that denaturating of the protein in the presence of SDS passes through both stages for a solution pH below the isoelectric point of the albumin, while the denaturing stops in the first stage for a solution pH above the isoelectric point of the albumin. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 5, pp. 661–665, September–October, 2006.     

Production of a chromium Bose–Einstein condensate

The recent achievement of Bose–Einstein condensation of chromium atoms [1] has opened longed-for experimental access to a degenerate quantum gas with long-range and anisotropic interaction. Due to the large magnetic moment of chromium atoms of 6 μ_B, in contrast to other Bose–Einstein condensates (BECs), magnetic dipole-dipole interaction plays an important role in a chromium BEC. Many new physical properties of degenerate gases arising from these magnetic forces have been predicted in the past and can now be studied experimentally. Besides these phenomena, the large dipole moment leads to a breakdown of standard methods for the creation of a chromium BEC. Cooling and trapping methods had to be adapted to the special electronic structure of chromium to reach the regime of quantum degeneracy. Some of them apply generally to gases with large dipolar forces. We present here a detailed discussion of the experimental techniques which are used to create a chromium BEC and allow us to produce pure condensates with up to 10⁵ atoms in an optical dipole trap. We also describe the methods used to determine the trapping parameters.     

Purification and fractionation of single-walled carbon nanotubes

This study presents the approach to the purification and subsequent metallic/semiconductive (M/S) fractionation of single-walled carbon nanotubes (SWCNTs) with diameter from 1.04 to 1.60 nm produced via laser ablation. SWCNTs were purified through 3-fold refluxing processes in nitric acid followed by the multiple washings with sodium hydroxide and hydrochloric acid. The purified-annealed SWCNTs sample was divided into seven batches. One batch was dispersed in acetone as a reference sample. Each of the remaining batches were dispersed in one of the following surface agents: sodium dodecyl sulfate, sodium cholate acid (SCA), sodium deoxycholate, cetrimonium bromide, cetylpyridinium chloride, and benzalkonium chloride (BKC). SWCNT suspensions were fractionated via free solution electrophoresis technique. The recovered fractions from electrode and control areas were analyzed via optical absorption spectroscopy in UV–Vis–NIR range to evaluate the efficiency of the separation process. Raman spectroscopy was applied to analyze the purity of the samples. The catalyst content was estimated by atomic absorption spectroscopy. The morphology of the investigated samples was observed via high-resolution transmission electron microscopy. This contribution clearly shows that among the investigated surfactants there are two promising candidates (SCA and BKC) which can efficiently enrich the bulk sample in one electronic type of carbon nanotubes when FSE is applied.     

Single step surface modification of highly stable magnetic nanoparticles for purification of His-tag proteins

The aim of this study was to develop a simple, cheap, and rapid method for purification of His-tag recombinant proteins with high yields. The new immobilized metal ion affinity adsorbent containing superparamagnetic nanoparticles and hydrophilic resins are proposed here to improve the purification of His-tagged recombinant proteins. In this report, we have described the preparation of nanosized superparamagnetic nanoparticles (Fe₃O₄) which were prepared by chemical precipitation method followed by surface modification using phosphonomethyl iminodiacetic acid. The stable surface functionalized nanoparticles were further linked with Ni²⁺ for purification of 6× His-tagged proteins. The phosphonate group of the N-phosphonomethyl iminodiacetic acid ligand acts as a surface anchoring agent on magnetite nanoparticles and the remaining free –COOH groups outside for binding with Ni²⁺ ions. The nanoparticles were approximately 6–8 nm in size and were stable and had negligible non-specific binding for protein. The proteins were purified within 1 h and observed on sodium dodecyl sulfate-polyacrylamide electrophoresis gel.     

Limited volume thin film deposition on geometrically complicated substrates

In this paper we report a study on the elastic scattering of electrons by lithium and sodium atoms in the presence of circularly polarized resonant laser field within the framework of the two-state rotating wave approximation. The effect of laser on projectile electrons is described by Volkov states. The frequency of the laser field is chosen to match with the 2s–3p (3s–3p) transition frequency in lithium (sodium) atoms. The total and differential elastic cross sections with single photon exchange are calculated for intermediate energies (50–150 eV) and laser intensity (10⁷–10¹¹ W cm^-2). An erratum to this article can be found online at http://dx.doi.org/. An erratum to this article can be found at     

Determination of the Constants of Binding of Acridine Dyes with Micelles of Sodium Dodecyl Sulfate Using the Quenching of Delayed Fluorescence by Heavy Atoms

The constants of binding dye molecules with the micelles of sodium dodecyl sulfate are determined using quenching of delayed fluorescence of acridine dyes by sodium iodide in aqueous–micellar solutions. Kinetic equations have been composed that describe the processes of deactivation of the excited states of dyes. By solving these equations at the concentration of the quencher sodium iodide corresponding to the minimum lifetime of triplet states and at the concentration of micelles corresponding to the least value of the delayed fluorescence quenching rate constants, we obtained the constants of binding dyes with micelles equal to 1.3·10⁷, 2.9·10⁷, and 3.1·10⁷ M^–1 for trypaflavine, acridine orange, and acridine yellow, respectively. We calculated the rate constants of quenching of the triplet states of the molecules of dyes by iodide ions (I ^–) that decreased in transition from trypaflavine to acridine orange and acridine yellow.     

Calculation of the vibrational spectrum of a sodium sulfate crystal

Based on model representations a calculation is made of the frequencies and forms of normal vibrations of a fragment of the sodium sulfate crystal in the third phase. Calculated results are compared to experimental RS spectra. Belarusian State University, 4, F. Skorina Ave., Minsk, 220050, Belarus. Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 66, No. 1, pp. 95–99, January–February, 1999.