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1.
Marcolan M Martins PA Pedrosa VA Rodrigues MR de Oliveira HP Codognoto L 《Journal of fluorescence》2011,21(2):733-738
A simple, rapid and effective analytical method based on fluorescence spectroscopy for the determination of coumarin in pharmaceutical
formulations without pre-treatment or pre-concentration step was development. Coumarin had maximum excitation and emission
at 310 nm and 390 nm, respectively. Optimum conditions for the detection of coumarin were investigated. Under optimized conditions,
we observed a linear behavior for the sign of coumarin in the concentration range of 2.5 × 10−6 to 1.0 × 10−4 mol L−1, with linearity of 0.998 and sensitivity of 2.9 × 1010 u.a/mol L−1. The proposed method was validated in terms of accuracy, precision and specificity of coumarin using the standard addition
and external calibration. It was noted that the results support (P < 0.05), indicating that the matrices were not an interference in the determination of coumarin by fluorescence spectroscopy.
The results were favorable compared with those obtained by reference chromatographic methods. 相似文献
2.
Quenching of fluorescence from Na(32
P) and K(42
P) atoms by various collision partners was studied at 973 and 1273K. Excited alkali atoms were produced photolytically by excimer
laser light at 193nm. For each collision pair, the appropriate relative velocity was computed and used to evaluate the quenching
cross-section from the measured rate constants. Cross sections for CO2, O2 and N2 are large (10–60Å2) while for Ar, the values are <1 Å2. The results are compared with those of previous investigations as a function of relative velocity. Finally, implications
for combustion diagnostics are briefly discussed.
Received: 29 March 1996 相似文献
3.
The binding of quercetin to lysozyme (LYSO) in aqueous solution was investigated by fluorescence spectroscopy, UV-vis absorption
spectroscopy and molecular simulation at pH 7.4. The fluorescence quenching of LYSO by addition of quercetin is due to static
quenching, the binding constants, K
a
, were 3.63 × 104, 3.31 × 104 and 2.85 × 104 L·mol−1 at 288, 298 and 308 K, respectively. The thermodynamic parameters, enthalpy change, ∆H, and entropy change, ∆S, were noted to be −7.56 kJ·mol−1 and 61.07 J·mol−1·K−1. The results indicated that hydrophobic interaction may play a major role in the binding process. The distance r between the donor (LYSO) and acceptor (quercetin) was determined as 3.34 nm by the fluorescence resonance energy transfer.
The synchronous fluorescence spectroscopy showed the polarity around the tryptophan residues increased and the hydrophobicity
decreased. Furthermore, the study of molecular simulation indicated that quercetin could bind to the active site (a pocket
made up of 24 amino-acid residues) of LYSO mainly via hydrophobic interactions and that there were hydrogen interactions between
the residues (Gln 57, Ile 98) of LYSO and quercetin. The accessible surface area (ASA) calculation verified the important
roles of tryptophan (Trp) residues during the binding process. 相似文献
4.
A new spectrofluorimetric method was developed for the determination of trace amounts of dopamine (DA). Using chlorosulfonylthenoyltrifluoroacetone
(CTTA)–europium ion (Eu3+) as a fluorescent probe, in a buffer solution at pH = 10.0, DA can remarkably enhance the fluorescence intensity of the CTTA-Eu3+ complex at λ = 612 nm; the enhanced fluorescence intensity of Eu3+ is proportional to the concentration of DA. Optimum conditions for the determination of DA were also investigated. The linear
range and detection limit for the determination of DA were 5.0 × 10−8∼1.6 × 10−5 mol/l and 3.2 × 10−8 mol/l. This method is simple, practical and relatively free of interference from coexisting substances, and can be applied
to assess DA in injection and human serum samples with good precision and accuracy. 相似文献
5.
The synthesis and functionalization of carbon nanoparticles with PEG200 and mercaptosuccinic acid, rendering fluorescent carbon dots, is described. Fluorescent carbon dots (maximum excitation and
emission at 320 and 430 nm, respectively) with average dimension 267 nm were obtained. The lifetime decay of the functionalized
carbon dots is complex and a three component decay time model originated a good fit with the following lifetimes: τ
1 = 2.71 ns; τ
2 = 7.36 ns; τ
3 = 0.38 ns. The fluorescence intensity of the carbon dots is affected by the solvent, pH (apparent pK
a of 7.4 ± 0.2) and iodide (Stern-Volmer constant of 78 ± 2 M−1). 相似文献
6.
J. Balogh D. Kaptás L. F. Kiss T. Kemény L. Bujdosó I. Vincze 《Hyperfine Interactions》2006,169(1-3):1343-1347
Magnetic multilayers of 57Fe with nominal thickness, T
nom, between 0.4 and 1.0 nm separated by 3.0 nm Al spacer layers were prepared by alternate deposition of the constituents in
high vacuum. The samples were investigated at 4.2 K in external magnetic field. A fraction of Fe atoms corresponding to about
0.3 nm equivalent Fe-thickness was found to mix into the Al spacer. The extremely strong magnetic anisotropy observed for
T
nom < 0.8 nm is attributed to Fe layers of approximately two atomic planes thick. The anisotropy decreases considerably after
the building up of the third Fe atomic layer starts at T
nom = 0.8 nm, but full saturation was not achieved even for T
nom = 1 nm and 3 T magnetic field applied perpendicularly to the sample plane. 相似文献
7.
Spectral properties of novel type of fluorophores consist of a π-conjugated system end-capped with an electron-donating N,N-dimethylaminophenyl group and an electron-withdrawing imidazole-4,5-dicarbonitrile moiety were examined. An additional π-linker
separating these two structural units comprises simple bond (B1P), phenyl (B2B), styryl (B3S) and ethynylphenyl (B4A) moieties.
The absorption and fluorescence spectra were taken in cyclohexane, chloroform, acetonitrile, methanol and in polymer matrices
such as polystyrene, poly(methyl methacrylate) and poly(vinylchloride). The longest-wavelength absorption band was observed
in the range of 300 to 400 nm. Intense fluorescence with quantum yields of 0.2 to 1.0 was observed in cyclohexane, chloroform
and in polymer matrices within the range of 380 to 500 nm. The fluorescence was strongly quenched in neat acetonitrile and
methanol. The fluorescence lifetimes are in the range of 1–4 ns for all measured fluorophores. The large Stokes shift (4,000
to 8,000 cm−1) indicates a large difference in the spatial arrangement of the chromophore in the absorbing and the emitting states. The
observed fluorescence of all fluorophores in chloroform was quenched by 1-oxo-2,2,6,6-tetramethyl-4-hydroxy piperidine by
the diffusion-controlled bimolecular rate (cca 2 × 1010 L mol−1 s−1). Polar solvents such as acetonitrile and methanol quenched the fluorescence as well but probably via a different mechanism. 相似文献
8.
The interaction between a classic uncoupler (2,4-dinitrophenol, DNP) and bovine serum albumin (BSA) was investigated by fluorescence
spectroscopy under the physiological conditions. The fluorescence quenching constants were calculated by the Stern-Volmer
equation, and based upon the temperature dependence of quenching constants, it was proved that DNP caused a static quenching
of the intrinsic fluorescence of BSA. Owing to the static quenching mechanism, different associative binding constants at
various temperatures were determined and thus the thermodynamic parameters, namely enthalpy (ΔH = −21.12 kJ mol−1) and entropy changes (ΔS = 23.51 J mol−1 K−1) could be calculated based on the binding constants. Moreover, the enthalpy and entropy changes are consistent with the “Enthalpy-Entropy
Compensation” equation obtained from our previous work. The negative enthalpy and positive entropy indicated that the electrostatic
interactions played a major role in DNP-BSA binding process. Site marker competitive displacement experiments were carried
out by using fluorescence and isothermal titration calorimetry (ITC) methods. These results showed that DNP bound with high
affinity to Sudlow’s site I (subdomain IIA) of BSA. The distance (r = 3.78 nm) between donor (BSA) and acceptor (DNP) was obtained according to the mechanism of fluorescence resonance energy
transfer (FRET). Furthermore, the results of synchronous fluorescence and circular dichroism (CD) spectroscopic studies indicated
that the microenvironment and the secondary conformation of BSA were altered. The above results were supported by theoretical
molecular modeling methods. 相似文献
9.
A rapid, simple and highly sensitive second derivative synchronous fluorometric method has been developed for the simultaneous
analysis of binary mixture of cinnarizine (CN) and domperidone (DOM). The method is based upon measurement of the native fluorescence
of these drugs at Δλ = 80 nm in aqueous methanol (50% V/V). The different experimental parameters affecting the native fluorescence
of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the
range of 0.1 to 1.3 μg mL−1 and 0.1–3.0 μg mL−1 for CN and DOM, respectively with lower detection limits of 0.017 and 5.77 × 10−3 μg mL−1 and quantification limits of 0.058 and 0.02 μg mL−1 for CN and DOM. The proposed method was successfully applied for the determination of the studied compounds in synthetic
mixtures and in commercial tablets. The results obtained were in good agreement with those obtained with reference methods.
The high sensitivity attained by the synchronous fluorometric method allowed the determination of CN in real and spiked human
plasma. The mean % recoveries in case of spiked human plasma (n = 3) were 96.39 ± 1.18 while that in real human plasma (n = 3) was 104.67 ± 4.16. 相似文献
10.
In this work, a new simple and sensitive flow injection method is developed for the determination of homocysteine with spectrofluorimetric
detection technique. This method is based on the oxidation of homocysteine with Tl (III) in acidic media, producing fluorescence
reagent, TlCl32- (λex = 237 nm, λem = 419 nm). The effects of chemical parameters (including pH of the solutions, the buffer, Tl (III) and potassium chloride
concentrations), instrumental parameters (such as flow rate of the solutions, reaction coil length, and sample loop volume)
and temperature on the fluorescence intensity as an analytical signal are studied and optimized. In the optimum conditions
of the above variables, homocysteine can be determined in the range 4.0 × 10-7–40.0 × 10-6 M with the LDR from 4.0 × 10-7 to 25.0 × 10-6 M. The detection limit (with S/N = 3) is 6.0 × 10-8 M of homocysteine and precision for the injection of 5.0, 10.0 and 15.0 μM of homocysteine are 0.8%, 1.5% and 2.5% (n = 10) respectively. The rate of analysis is 90 samples per hour. The influence of potential interfering substances, including
amino acids and carbohydrates is also studied. The proposed method has been successfully used for the determination of homocysteine
in the real sample (blood serum and tap water) matrix. 相似文献
11.
Irmina Herburt 《Mathematical Physics, Analysis and Geometry》2007,10(3):251-259
The dual volume of order α of a convex body A in R
n
is a function which assigns to every a ∈ A the mean value of α-power of distances of a from the boundary of A with respect to all directions. We prove that this function is strictly convex for α > n or α < 0 and strictly concave for 0 < α < n (for α = 0 and for α = n the function is constant). It implies that the dual volume of a convex body has the unique minimizer for α > n or α < 0 and has the unique maximizer for 0 < α < n. The gravitational centre of a convex body in R3 coincides with the maximizer of dual volume of order 2, thus it is unique.
相似文献
12.
In our study, terbium-acetylacetone (Tb-acac) composite nanoparticles have been prepared under vigorous ultrasonic irradiation.
The nanoparticles are water soluble, stable and have extremely narrow emission bands and high internal quantum efficiencies.
They were used as fluorescence probes in the determination of enoxacin (Enox) based on the fluorescence enhancement of nanoparticles
through fluorescence resonance energy transfer (FRET). The influence of buffer solution on the fluorescence intensity was
investigated. Under the optimum conditions, the fluorescence intensity of the Tb-acac-Enox system is linearly proportional
to the Enox concentration in the Enox concentration range of 2 × 10−7–1 × 10−4 M. The correlation coefficient for the calibration curve was 0.9976. The limit of detection as defined by IUPAC, C
LOD = 3S
b/m (where S
b is the standard deviation of the blank signals and m is the slope of the calibration graph) was found to be 3 × 10−8 M. The relative standard deviation (RSD) for six repeated measurements of 1 × 10−4 M Enox was 1.35%. The method was applied to the determination of Enox in pharmaceutical formulation and recovery results
were obtained from urine samples. 相似文献
13.
Luteolin and apigenin, extracted from Reseda luteola L., were spectrophotometrically and fluorimetrically studied. The spectra were investigated as a function of pH in methanol/water
solutions (1/2, v/v) in the 2–12 pH range. The absorption spectra markedly shifted to the red by increasing the pH. Three acid–base dissociation
steps were detected for luteolin (pK
a = 6.9; 8.6; 10.3) and two for apigenin (pK
a = 6.6; 9.3). Fluorescence emission was very weak or undetectable (Φ
F < 10−4) in acidic solution, but increased in intensity with increasing the pH. Both molecules exhibited a great propensity towards
complex formation with metal ions, with association constants on the order of 105–107 for the first complexation step; in the presence of excess Al3+ ions, multiple equilibria were detected. A marked fluorescence enhancement was observed upon complexation with Al3+ ions (Φ
F ∼ 1 for luteolin and ∼10−2 for apigenin). 相似文献
14.
The interaction of a N-methylated diaminotriphenylmethane dye, malachite green, with lysozyme was investigated by fluorescence spectroscopic techniques
under physiological conditions. The binding parameters have been evaluated by fluorescence quenching methods. The results
revealed that malachite green caused the fluorescence quenching of lysozyme through a static quenching procedure. The thermodynamic
parameters like ΔH and ΔS were calculated to be −15.33 kJ mol−1 and 19.47 J mol−1 K−1 according to van’t Hoff equation, respectively, which proves main interaction between malachite green and lysozyme is hydrophobic
forces and hydrogen bond contact. The distance r between donor (lysozyme) and acceptor (malachite green) was obtained to be 3.82 nm according to Fӧrster’s theory. The results
of synchronous fluorescence, UV/vis and three-dimensional fluorescence spectra showed that binding of malachite green with
lysozyme can induce conformational changes in lysozyme. In addition, the effects of common ions on the constants of lysozyme-malachite
green complex were also discussed. 相似文献
15.
In pH 1.8 ∼ 2.8 weak acid medium, polyvinylpyrrolidone (PVP) and Eosin Y reacted to form complex that could result in Eosin
Y (EY) fluorescence quenching. The maximum quenching wavelength was at 542 nm. The fluorescence quenching (ΔF) was proportional to the concentration of polyvinylpyrrolidone in a certain range. The linear range, the correlation coefficient
and the detection limit were 0.33 ∼ 2.0 μg•mL−1, 0.9994 and 99.6 ng•mL−1, respectively. The influences of the coexistence substances were tested and the results showed that the method had good selectivity.
Therefore, a new method based on fluorescence quenching of eosin Y by PVP for the determination of trace PVP was developed.
The method was sensitive, simple and rapid, which was applied to the determination of trace PVP in the beer with satisfactory
results. The reaction mechanism was also discussed. 相似文献
16.
P. J. Ramesh K. Basavaiah N. Rajendraprasad O. Zenita Devi K. B. Vinay 《Journal of Applied Spectroscopy》2011,78(3):383-391
Two simple spectrophotometric methods have been developed to analyze ofloxacin (OFX) in pharmaceuticals. The methods are based
on the oxidation of OFX by a measured excess of cerium(IV) sulfate in H2SO4 medium. This was followed by the determination of the unreacted oxidant by reacting it with either p-toluidine (p-TD) and measuring the absorbance at 525 nm (method A) or o-dianisidine (o-DA) and measuring the absorbance at 470 nm (method B). In both methods, the amount of cerium(IV) sulfate reacted corresponds
to the amount of OFX. Calibration graphs were linear over the ranges of 0–120 and 0–4 g/ml OFX for methods A and B, respectively.
The calculated molar absorptivity (2.34⋅103 and 5.99⋅104), Sandell sensitivity, and limit of quantification for the methods are reported. The intra-day precision (%RSD) and accuracy
(%RE) were < 8.0 and ≤ 4.0%, respectively, and the inter-day RSD and RE values were within 5 and 4.0%, respectively. The applicability
of the methods was demonstrated by determining OFX in tablets with an accuracy (%RE) of < 3% and precision (%RSD) of ≤2.65%.
The accuracy of the methods was further ascertained by recovery experiments via a standard-addition procedure. 相似文献
17.
This paper explores an ultra-sensitive luminescence method for the determination of Ketoprofen (KP) in pharmaceutical formulations.
The technique is indirect and exploits the luminescence enhancement of terbium (Tb3+) by complexation with KP (Tb3+–KP), which was monitored at respective excitation and emission wavelengths of λ
ex = 258 nm and λ
em = 549 nm. The effect of varying the Tb3+ concentration and using multiple solvents was examined to determine optimal experimental conditions. Maximum sensitization
was accomplished in the presence of methanol where the most favourable condition for the formation of the complex was recorded
at a level of 1.0 × 10−5 M of Tb3+. Under these optimum experimental conditions, linear calibration curve was obtained in the range of 2.8 × 10−7–3.1 × 10−6 M with a detection limit of 8.7 × 10−8 M. The technique was validated with ‘working’ reference standards and produced relative standard deviations < 2% indicating
that the reproducibility was highly acceptable. The proposed method was successfully applied to assays of KP in pharmaceutical
formulations with average recoveries of 92–98%. The results were found to be in good agreement with those obtained by HPLC.
The method is highly suited for general applications of this nature. 相似文献
18.
The saccharide binding and conformational characterization of a hemagglutinin, a low molecular weight protein from the seeds
of Moringa oleifera was studied using steady state and time resolved fluorescence. The lectin binds sugars LacNAc (K
a = 1380 M−1) and fructose (K
a = 975 M−1), as determined by the fluorescence spectroscopy. It has a single tryptophan per monomer which is exposed on the surface
and is in a strong electropositive environment as revealed by quenching with iodide. Quenching of the fluorescence by acrylamide
involved both static (K
s = 0.216 M−1) and collisional (K
sv = 8.19 M−1) components. The native protein showed two different lifetimes, τ
1 (1.6 ns) and τ
2 (4.36 ns) which decrease and get converted into a single one, (2.21 ns) after quenching with 0.15 M acrylamide. The bimolecular
quenching constant, k
q
was 7.55 × 1011 M−1 s−1. ANS binding studies showed that the native protein has exposed hydrophobic patches which get further exposed at extreme
acidic or alkaline pH. However, they get buried in the interior of the protein in presence of 1 M GdnHCl or urea. 相似文献
19.
The interaction between thyroxine hormone and 7 hydroxycoumarin (7HC) was investigated using fluorescence quenching method.
The experimental results showed that thyroxine could quench the fluorescence of 7HC by forming the 7HC–thyroxine complex with
static quenching. The apparent binding constants (K) between 7HC and thyroxine were determined to be 1.51 × 104 (297 K) and 9.06 × 103 (310 K). The binding sites (n) 0.98 ± 0.1. The thermodynamic parameters showed that the interaction between 7HC and thyroxine was driven mainly by hydrogen
bonding interactions and van der Waals force. Calibration for thyroxine, based on quenching titration data, was linear in
the concentration range 2.0 × 10−8 to 3.0 × 10−7 mol/l. The relative standard deviation was 2.58% for 2.0 × 10−7 mol/l thyroxine (n = 4) and the 3σ limit of detection was 3.42 × 10−8 mol/l in cationic surfactant CTAB medium. 相似文献
20.
A sensitive and selective method for the trace determination of 3, 3’, 4, 4’-tetrachlorobiphenyl (PCB77) by using bovine serum
albumin (BSA) as a fluorescence probe was introduced. Under optimum conditions, the enhanced fluorescence intensity was proportional
to the concentration of polychlorinated biphenyls in the range of 8.9 × 10−8–5.0 × 10−6 mol L−1 for PCB77, and 5.0 × 10−7–5.0 × 10−6 mol L−1 for 2, 2’, 5, 5’-tetrachlorbiphenyl (PCB52). The detection limits (S/N = 3) of PCB77 and PCB52 were 2.6 × 10−8 mol L−1 and 2.9 × 10−7 mol L−1, respectively. Furthermore, the fluorescence enhancement mechanism was discussed in detail. Results indicated that fluorescence
enhancement of the system originated from the formation of BSA-PCBs complexes. In addition, PCBs were mainly bound to the
tyrosine residues in BSA molecules. 相似文献