Determination of albumins by its quenching effect on the fluorescence of Tb-oxolinic acid complex in presence of sodium dodecyl sulphate

It is found that the fluorescence intensity of Tb³⁺-oxolinic acid (OA) complex can be greatly quenched by albumins in sodium dodecyl sulphate (SLS). Under optimum conditions, the quenched fluorescence intensity is in proportion to the concentration of proteins in the range of 5.0×10⁻⁸-1.0×10⁻⁵ g ml⁻¹ for bovine serum albumin (BSA), 1.0×10⁻⁷-1.0×10⁻⁵ g ml⁻¹ for human serum albumin (HSA) and 4.0×10⁻⁷-1.0×10⁻⁵ g ml⁻¹ for egg albumin (EA). Their detection limits (S/N=3) are 2.1×10⁻⁸, 2.5×10⁻⁸ and 5.0×10⁻⁸ g ml⁻¹, respectively. In addition, the interaction mechanism is also investigated.     

Conducting polymer film-based immunosensors using carbon nanotube/antibodies doped polypyrrole

Carbon nanotube/polypyrrole/antibodies polymer films were synthesized successfully on microelectrodes by electrochemical deposition. Electropolymerization was performed at optimal range between −0.8 and +0.8 V at a scan rate of 50 mV s⁻¹ in an electrochemical mini-cell containing monomer pyrroles, carbon nanotubes, and goat IgGs. The conducting polymer films were characterized by Fourier transform infrared spectrometry, Raman spectra, and Field emission scanning electron microscopy. And then, it was prepared for immunosensor application to determine anti-goat IgGs. The results show that a linear range between 0.05 and 0.7 μg ml⁻¹ for anti-goat IgGs detection was observed for immunosensor, a detection limit as low as 0.05 μg ml⁻¹ and a response time of 1 min. The effect parameters of electropolymerization process on immunosensor response are also studied. It found that the immunosensor well active in 1.5 mg ml⁻¹ CNT concentration, 2.5 mM pyrrole, 10 μg ml⁻¹ goat IgGs.     

Synthesis and luminescence properties of lanthanide(III) chelates with polyacid derivatives of thienyl-substituted terpyridine analogues

Two new polyacid derivative ligands of thienyl-substituted terpyridine analogues, N,N,N¹,N¹-[4′-(2?-thienyl)-2,2′:6′,2″-terpyridine-6,6″-diyl]bis(methylenenitrilo) tetrakis(acetic acid) (TTTA) and N,N,N¹,N¹-[2,6-bis(3′-aminomethyl-1′-pyrazolyl)-4-(2″-thienyl)pyridine] tetrakis(acetic acid) (BTTA), were synthesized, and the luminescence properties of their Eu³⁺ and Tb³⁺ chelates were investigated. The Eu³⁺chelates of the two ligands are strongly luminescent having luminescence quantum yields of 0.150 (TTTA-Eu³⁺) and 0.114 (BTTA-Eu³⁺), and lifetimes of 1.284 ms (TTTA-Eu³⁺) and 1.352 ms (BTTA-Eu³⁺), whereas their Tb³⁺ chelates are weakly luminescent. The TTTA-Eu³⁺ chelate was used for streptavidin (SA) labeling, and the labeled SA was used for time-resolved fluoroimmunoassay of insulin in human sera. The method gives the detection limits of 33 pg ml⁻¹.     

A simple fluorescence quenching method for roxithromycin determination using CdTe quantum dots as probes

A new method for the determination of roxithromycin based on the fluorescence quenching of 3-mercaptopropionic acid-capped CdTe quantum dots (MPA-CdTe QDs) was developed. In ethanol medium, the fluorescence of CdTe quantum dots at 552 nm was quenched in the presence of roxithromycin. Based on this a simple, sensitive, and selective method for rapid determination of roxithromycin was described. Reaction time, interfering substances on the fluorescence quenching, and mechanism of the interaction of CdTe QDs with roxithromycin were investigated. After optimization, the proposed method allows the determination of roxithromycin over the range 25.0-350.0 μg ml⁻¹. The detection limit is 4.6 μg ml⁻¹. The proposed method was successfully applied to commercial capsules and tablets with satisfactory results. The recovery of the method was in the range of 96.8-102.5%.     

Determination of the refractive index over a wide wavelength range through time-delay measurements of femtosecond pulses

We present a simple method to measure the refractive index dispersion over a broad wavelength range (0.6-1.6 μm). In a first step, the optical group indices are obtained by measuring the time-retardation of tunable 150 fs laser pulses within a sample relative to air. The refractive index dispersion is then calculated using a Sellmeier equation that describes the measured group index dispersion. We show that our experimental data agree with previously published results to within 2 × 10⁻⁴ for a 3 mm thick sample of fused silica and to within 3 × 10⁻³ for the index n₁ of a 2 mm thick crystal of the highly dispersive and anisotropic organic crystal 4-N,N-dimethylamino-4′-N′-methyl stilbazolium tosylate (DAST).     

Designing of endlessly single mode polarization maintaining highly birefringent nonlinear micro-structure fiber at telecommunication window by FV-FEM

An endlessly single mode highly polarization maintaining nonlinear microstructure fiber at telecommunication window is reported via full-vector finite element method. By taking three ring hexagonal PCF with suitable fiber parameter such as air hole diameter in cladding region d = 0.8 μm, pitch 2.3 μm and introducing four symmetrical large air holes near core region d′ = 2 μm, single mode (V_eff ≤ π), small effective mode area 2.7 μm², nonlinear co-efficient 44.39 W⁻¹ km⁻¹, high phase birefringence of the order of 10⁻³ and group birefringence of the order of 10⁻⁴ with beat length 0.3 μm at wavelength 1.55 μm are achieved.     

Measurements of optical parameters of phantom solution and bulk animal tissues in vitro at 650 nm

Optical parameters of bulk animal tissue in vitro, including absorption coefficient (μ_a), reduced scattering coefficient (μ′_s) or scattering coefficient (μ_s), total attenuation coefficient (μ_t), anisotropy factor (g) and refractive index (n) are measured at wavelength of 650 nm. Clinical Intralipid-10% is diluted in distilled water into different concentrations to use as tissue phantoms. Four types of animal tissues in vitro are studied. The relationships among the optical parameters are analyzed systemically. For animal tissues, μ_a, μ′_s or μ_s and n rely on muscle fiber orientations. μ_s and μ_t range from 10 to 20 mm⁻¹, μ_a from 10⁻² to 10⁻³ mm⁻¹ and g from 0.95 to 0.99.     

Colorimetric microdetermination of captopril in pure form and in pharmaceutical formulations

A simple, rapid, accurate, precise and sensitive colorimetric method for the determination of captopril (CAP) in bulk sample and in dosage forms is described. The method is based on oxidation of the drug by potassium permanganate in acidic medium and determination of the unreacted oxidant by measuring the decrease in absorbance for five different dyes; methylene blue (MB); acid blue 74 (AB), acid red 73 (AR), amaranth dye (AM) and acid orange 7 (AO) at a suitable λ_max (660, 610, 510, 520, and 485 nm), respectively. Regression analysis of Beer's plots showed good correlation in the concentration ranges (0.4-12.5, 0.3-10, 0.5-11, 0.4-8.3 and 0.5-9.3 μg ml⁻¹), respectively. The apparent molar absorbtivity, Sandell sensitivity, detection and quantitation limits were calculated. For more accurate results, Ringbom optimum concentration ranges were 0.5-12, 0.5-9.6, 0.6-10.5, 0.5-8.0 and 0.7-9.0 μg ml⁻¹, respectively. The validity of the proposed method was tested by analyzing in pure and dosage forms containing CAP whether alone or in combination with hydrochlorothiazide. Statistical analysis of the results reflects that the proposed procedures are precise, accurate and easily applicable for the determination of CAP in pure form and in pharmaceutical preparations. Also, the stability constant was determined and the free energy change was calculated potentiometrically.     

Direct observation of the D′ 2g(P2)-A′ Π(2u) system for Cl2 by laser induced fluorescence spectroscopy: Determination of the absolute position of the A′ state

In a discharged supersonic jet of Cl₂, transitions of the D′ 2_g(³P₂)-A′ ³Π(2_u) system for ³⁵Cl₂ were observed directly by laser induced fluorescence spectroscopy. By a discharge in Cl₂, the Cl₂ molecules were populated into the A′ state, which is a metastable and optically forbidden state, from the state. An ultraviolet laser radiation excites the molecules to the D′ ion-pair state. A set of Dunham parameters for the A′ state is determined from a global least-squares fitting for 59 vibronic bands with v″ = 0-7. In the fitting, the previously reported data, T(v) and B(v) for the v = 14 and 15 bands of the A′ state [T. Ishiwata, A. Ishiguro, K. Obi, J. Mol. Spectrosc. 147 (1991) 300-320], were included. Y₀₀ = 57295.723(5) cm⁻¹ of the D′ state [J.-H. Si, T. Ishiwata, K. Obi, J. Mol. Spectrosc. 147 (1991) 334-345] was also included in the global fitting in order to determine the absolute position of the A′ state. The determined parameters of the A′ state are Y₀₀ = 17171.506(14), Y₁₀ = 255.915(85), Y₂₀ = −4.465(70), Y₃₀ = −8.7(23) × 10⁻², Y₄₀ = 6.3(35) × 10⁻³, Y₅₀ = −4.9(26) × 10⁻⁴, Y₆₀ = 1.43(69) × 10⁻⁵, Y₀₁ = 0.16282(15), Y₁₁ = −2.363(68) × 10⁻³, Y₂₁ = −5.01(93) × 10⁻⁵, and Y₃₁ = −3.01(36) × 10⁻⁶ (in cm⁻¹ and one standard deviations of the fit in parentheses). The absolute position of the A′ state is determined with good accuracy.     

Preparation of a novel fluorescence probe of terbium-europium co-luminescence composite nanoparticles and its application in the determination of proteins

Terbium-europium Tb-Eu/acetylacetone(acac)/poly(acrylamide) (PAM) co-luminescence composite nanoparticles were successfully prepared using the ultrasonic approach. The as-prepared composite nanoparticles show the characteristic emission spectra of Tb³⁺, located at 496 and 549 nm. Furthermore, the nanoparticles are water soluble, stable and have extremely narrow emission bands and high internal fluorescence quantum yield due to the co-luminescence effect. Further studies indicate that proteins can interact with the nanoparticles and induce the fluorescence quenching of the nanoparticles. Based on the fluorescence quenching of nanopaticles in the presence of proteins, a novel method for the sensitive determination of trace amounts of proteins was proposed. Under the optimal experimental conditions, the linear ranges of calibration curves are 0-3.5 μg mL⁻¹ for human serum albumin (HSA) and 0-4.0 μg mL⁻¹ for γ-globulin (γ−IgG), respectively. The limits of detection are 7.1 for HSA and 6.7ng mL⁻¹ for γ−IgG, respectively. The method was applied to the quantification of proteins in synthetic samples and actual human serum samples with satisfactory results. This proposed method is sensitive, simple and has potential application in the clinical assay of proteins.     

Doppler-limited CW infrared cavity ringdown spectroscopy of the ν1+ν3 OH + CH stretch combination band of jet-cooled methanol

A high resolution cavity ringdown spectrometer (CRDS) has been constructed using a 1.5 μm continuous-wave external-cavity tunable diode laser, a mode-matched near-confocal ringdown cavity, and 2 cm pulsed slit jet. Without signal averaging, the RMS noise in the absorption signal is 1.7 × 10⁻⁹ cm⁻¹. The rotationally resolved overtone spectrum of the OH(ν₁) + CH(ν₃) stretch combination band of methanol between 6510 and 6550 cm⁻¹ has been observed for J^′=0-8 and K^′=0-3 at sub-Doppler resolution. In total, 418 lines are assigned and global fits yield molecular torsion-rotation parameters for the upper state. Four K^′-localized perturbations are analyzed and the pattern of residuals is discussed.     

Measurements and theoretical calculations of N2-broadening and N2-shift coefficients in the ν2 band of CH3D

In this paper, we report measured Lorentz N₂-broadening and N₂-induced pressure-shift coefficients of CH₃D in the ν₂ fundamental band using a multispectrum fitting technique. These measurements were made by analyzing 11 laboratory absorption spectra recorded at 0.0056 cm⁻¹ resolution using the McMath-Pierce Fourier transform spectrometer located at the National Solar Observatory on Kitt Peak, Arizona. The spectra were obtained using two absorption cells with path lengths of 10.2 and 25 cm. The total sample pressures ranged from 0.98 to 402.25 Torr with CH₃D volume mixing ratios of 0.01 in nitrogen. We have been able to determine the N₂ pressure-broadening coefficients of 368 ν₂ transitions with quantum numbers as high as J″ = 20 and K = 16, where K″ = K′ ≡ K (for a parallel band). The measured N₂-broadening coefficients range from 0.0248 to 0.0742 cm⁻¹ atm⁻¹ at 296 K. All the measured pressure-shifts are negative. The reported N₂-induced pressure-shift coefficients vary from about −0.0003 to −0.0094 cm⁻¹ atm⁻¹. We have examined the dependence of the measured broadening and shift parameters on the J″, and K quantum numbers and also developed empirical expressions to describe the broadening coefficients in terms of m (m = −J″, J″, and J″ + 1 in the ^QP-, ^QQ-, and ^QR-branch, respectively) and K. On average, the empirical expressions reproduce the measured broadening coefficients to within 4.7%. The N₂-broadening and pressure-shift coefficients were calculated on the basis of a semiclassical model of interacting linear molecules performed by considering in addition to the electrostatic contributions the atom-atom Lennard-Jones potential. The theoretical results of the broadening coefficients are in good overall agreement with the experimental data (8.7%). The N₂-pressure shifts whose vibrational contribution is derived from parameters fitted in the ^QQ-branch of self-induced shifts of CH₃D, are also in reasonable agreement with the scattered experimental data (20% in most cases).     

High resolution infrared spectroscopy of [1.1.1]propellane

The infrared spectrum of [1.1.1]propellane has been recorded at high resolution (0.002 cm⁻¹) with individual rovibrational lines resolved for the first time. This initial report presents the ground state constants for this molecule determined from the analysis of five of the eight infrared-allowed fundamentals ν₉(e′), ν₁₀(e′), ν₁₂(e′), , as well as of several combination bands. In nearly all cases it was found that the upper states of the transitions exhibit some degree of perturbation but, by use of the combination difference method, the assigned frequencies provided over 4000 consistent ground state difference values. Analysis of these gave for the parameters of the ground state the following values, in cm⁻¹: B₀ = 0.28755833(14), D_J = 1.1313(5) × 10⁻⁷, D_JK = −1.2633(7) × 10⁻⁷, H_J = 0.72(4) × 10⁻¹³, H_JK = −2.24(13) × 10⁻¹³, and H_KJ = 2.25(15) × 10⁻¹³, where the numbers in parentheses indicate twice the uncertainties in the last quoted digit(s) of the parameters. Gaussian ab initio calculations, especially with the computed anharmonic corrections to some of the spectroscopic parameters, assisted in the assignments of the bands and also provided information on the electron distribution in the bridge-head carbon-carbon bond.     

Preparation and microwave-absorbing properties of NiFe2O4-polystyrene composites

NiFe₂O₄ nanoparticles were synthesized by the polyacrylamide gel method with acrylamide as the monomer and N,N′-methylenediacrylamide as lattice agent. The average crystallite sizes of the nickel ferrites annealed at 500, 600 and 800 °C are about 10, 30 and 50 nm, respectively. Ferrite-polystyrene composites were made by hot pressing, and microwave-absorbing properties of the composites with different contents of 35, 45, 55 and 65 wt% ferrite were investigated by testing complex permeability and complex permittivity in the X-band (8.2-12.4 GHz) frequency range. All the parameters, ε′, ε″, μ′ and μ″, increase with increasing ferrite content. The reflection losses were calculated based on a model of a single-layered plane wave absorber backed by a perfect conductor. The composite with 65 wt% ferrite content shows a minimum reflection loss of −13 dB at 11.5 GHz with a −10 dB bandwidth over the extended frequency range of 10.3-13 GHz for an absorber thickness of 2 mm.     

Preconcentration of middle oxyethylated nonylphenols from water samples on magnetic solid phase

Magnetic solid phase extraction (MSPE) is proposed as a simple and fast method for the preconcentration of free middle oxyethylated nonylphenols (NPs) from water. Middle oxyethylated NPs were extracted by MSPE from different water samples (10 and 500 ml samples of distilled, potable, well, river and pond water in concentrations of 30 and 0.6 μg ml⁻¹) using magnetically modified polyphenyleneoxide, Tenax TA and Tenax GR as magnetic adsorbents. Recoveries were 80–100% and relative standard deviations were less than 10%.     

Structure and high pressure behaviour of organic crystals based on aromatically substituted 1,3,4-oxadiazoles

The crystalline structure of a new compound containing the 1,3,4-oxadiazole moiety, 4-(5-methyl-1,3,4-oxadiazole-2yl-)-N,N′-dimethyl-phenylamine (MODPA) was determined. It shows a monoclinic structure with space group P2₁/c and lattice parameters: a=1.02997(6), b=0.64840(4), c=1.58117(10) nm and β=99.4820(10)°. To study the intermolecular interactions in oxadiazole containing organic crystals, X-ray studies on MODPA and 2,5-diphenyl-1,3,4-oxadiazole (DPO) were performed up to 5 GPa at room temperature. The Murnaghan equation of state is used to describe the compression behaviour of both substances. From these results, the bulk modulus and its pressure derivative were determined. The values obtained are: K₀=6.3 GPa and K′₀=6.8 for MODPA and K₀=7.3 GPa and K′₀=6.7 for DPO. Additionally, measurements under increasing temperature at ambient pressure were carried out to evaluate the thermal expansion coefficient: α=1.8×10⁻⁴ K⁻¹ for MODPA and α=1.9×10⁻⁴ K⁻¹ for DPO.     

Deposition and electrostatic removal of gaseous organic contaminants on substrate surfaces

The adhesion behavior of di-n-butyl phthalate (DBP) onto different substrates (quartz, glass, and silicon) used as wafer surfaces was studied by using an in situ UV spectrophotometric technique. The results from the closed cell experiments revealed that greatest extent of DBP adhesion occurred on the quartz chip (0.154 μg cm⁻²), followed in the order by the glass (0.054 μg cm⁻²) and silicon (0.039 μg cm⁻²). By means of the in situ spectrophotometric observation, application of an electrical field at 290 V cm⁻¹ in the cell proved to be effective in inducing charging of DBP aerosols, which were consequently attracted towards the electrodes. This method can be applied to wafer storage and transport equipments to prevent wafer contamination from material outgassing representative by DBP.     

Fourier transform spectroscopy of N2O weak overtone transitions in the 1-2 μm region

The absorption spectrum of the natural sample of nitrous oxide has been recorded at Doppler limited resolution with a Fourier-transform spectrometer in the spectral range 5000-10 000 cm⁻¹. Ten cold bands (8Σ − Σ and 2Σ − Π), thirteen hot bands (11Π − Π, Σ − Σ, and Δ − Δ) of ¹⁴N₂¹⁶O and the 3ν₃ band of ¹⁴N¹⁵N¹⁶O have been newly detected. The uncertainty of the line position determination is estimated to be about 0.005 cm⁻¹ for unblended lines. The assignment of the spectrum has been done with the help of the prediction performed within the framework of the polyad model of effective Hamiltonian. The spectroscopic parameters G_v, B_v, D_v, H_v, and q_v have been determined for all newly detected bands. The line intensities of 13 weak bands have been measured. The uncertainty of the obtained line intensity values varies from 7 to 13%.     

Observation of fast sound in metal-nonmetal transition in liquid Hg

Liquid Hg undergoes the metal-nonmetal (M-NM) transition when it is expanded from 13.6 g cm⁻³ at ambient conditions to 9 g cm⁻³ at high temperature and high pressure. To investigate collective and single particle motions in expanded fluid Hg, we have made inelastic X-ray scattering experiments and obtained the dynamic structure factor, S(Q,ω), of fluid Hg. We analyzed S(Q,ω) within the framework of generalized hydrodynamics and found that the excitation energies of collective modes disperse three times as fast as the hydrodynamic sound velocity in the M-NM transition region at 9 g cm⁻³. The results indicate the existence of fast sound in expanded fluid Hg accompanying the metal-non-metal transition and strongly hint that fluctuations intrinsic to the M-NM transition are induced on atomic length scale and sub-picosecond time scale.     

Experimental determination of pressure-broadening parameters of millimeter-wave transitions of HNO3 perturbed by N2 and O2, and of their temperature dependences

We report on linewidth measurements on the J=24_K,11−23_K^′,10 and J=38_K,33−37_K^′,32 millimeter wave transitions in the ground vibrational state of nitric acid, located near 470.23 and 544.36 GHz, respectively. Experiments were performed with N₂ and O₂ as perturber molecules, in the 240-350 K temperature range by using a video-type spectrometer. The foreign-gas broadening parameters and their temperature dependence coefficients were determined using the Voigt profile, no narrowing effect being observed. In order to check the reliability of reported values, we carried out measurements on the J=14_K,12−13_K^′,11 transition located near 206.6 GHz, previously observed in two other laboratories. For this last line all the reported values are consistent themselves within one claimed standard deviation.