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1.
A new, simple, sensitive and selective spectrofluorimetric method for the determination of Hydrochlorothiazide was developed in acetonitrile at pH 6.2. The Hydrochlorothiazide can remarkably enhance the luminescence intensity of the Tb3+ ion doped in sol–gel matrix at λex = 370 nm. The intensity of the emission band of Tb3+ ion doped in sol–gel matrix was increased due to the energy transfer from the triplet excited state of Hydrochlorothiazide to (5D4) excited energy state of Tb3 ion. The enhancement of the emission band of Tb3+ ion doped in sol–gel matrix at (5D47 F5) 545 nm was directly proportion to the concentration of Hydrochlorothiazide with a dynamic ranges of 5.0 × 10−10—5.0 × 10−6 mol L−1 and detection limit of 2.2 × 10−11 mol L−1.  相似文献   

2.
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   

3.
In the paper, a chemiluminescence (CL) system was developed based on the catalytical effect of diperiodatocuprate (III) (DPC) on the 1,10-phenanthroline (phen)/hydrogen peroxide (H2O2) in the presence of cetyltrimethylammonium bromide (CTAB). The effects of experimental conditions were investigated. Meanwhile the increase of CL intensity of the DPC/phen/H2O2/CTAB system is proportional to the concentration of phen in the range of low concentration. The linear range of the calibration curve is 5.0 × 10−9–1.0 × 10−6 mol L−1, and the corresponding detection limit is 1.9 × 10−9 mol L−1. The effects of phenolic compounds (PCs) on the system were investigated. Hydroquinone was used as an example to investigate the application of the CL system to the determination of PCs. The quenched CL intensity is linearly related to the logarithm of concentration of hydroquinone. The linear range of the calibration curve is 2.5 × 10−9–1.0 × 10−5 g mL−1, and the corresponding detection limit is 1.8 × 10−9 g mL−1. This phen and hydroquinone can be synchronously determined. The method was applied to the determination of hydroquinone in water samples and the recoveries were from 92% to 106%.  相似文献   

4.
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   

5.
A simple and sensitive spectrofluorimetric method for determination of trace amount of doxycycline hydrochloride (DC) in pharmaceutical tablets and serum samples was developed. In ammonia buffer solution of pH 8.9 the doxycycline hydrochloride can remarkably enhance the luminescence intensity of the Sm3+ ion in Sm3+- DC complex at λex = 400 nm. The produced luminescence intensity of Sm3+- DC complex in DMSO is in proportion to the concentration of DC and used as optical sensor for its determination. The dynamic range for the determination of DC is 1 × 10−8 – 5 × 10−6 mol L−1 and in case of quantum yield calculations is 7 × 10−9 – 5 × 10−6 mol L−1 with detection limit of 6.5 × 10−10 mol L−1. The enhancement mechanism of the luminescence intensity in the Sm3+- DC system has been also discussed. A comparison with other spectrofluorimetric methods for tetracycline derivatives in which Eu3+ ion is used instead of Sm3+ ion is also studied.  相似文献   

6.
A rapid, simple and sensitive spectrofluorimetric method for determination of trace amount of ofloxacin was developed. At pH 5.1 the ofloxacin enhances the luminescence intensity of the Eu3+ ion in Eu3+- ofloxacin complex at λex = 365 nm. The produced luminescence intensity of Eu3+-ofloxacin complex was in proportional to the concentration of ofloxacin. The working range for the determination of ofloxacin was 5.0 × 10-9–5.0 × 10-6 mol L-1 with lower detection limit (LOD) and quantitative detection limit (QDL) of 3 × 10-9 and 9 × 10-9 mol L-1, respectively. The enhancement mechanism of the luminescence intensity in the Eu3+-ofloxacin system has been also explained. The method revealed good selectivity for ofloxacin in the presence of coexisting substances and used successfully for the assay of ofloxacin in pharmaceutical preparations and serum. A comparison with other standard methods was also discussed.  相似文献   

7.
Water-soluble Mn2+-doped ZnS quantum dots (QDs) were prepared using mercaptoacetic acid as the stabilizer. The optical properties and structure features were characterized by X-Ray, absorption spectrum, IR spectrum and fluorescence spectrum. In pH 7.8 Tris-HCl buffer, the QDs emitted strong fluorescence peaked at 590 nm with excitation wavelength at 300 nm. The presence of sulfide anion resulted in the quenching of fluorescence and the intensity decrease was proportional to the S2− concentration. The linear range was from 2.5 × 10−6 to 3.8 × 10−5 mol L−1 with detection limit as 1.5 × 10−7 mol L−1. Most anions such as F, Cl, Br, I, CH3CO2 , ClO4 , CO3 2−, NO2 , NO3 , S2O3 2−, SO3 2− and SO4 2− did not interfere with the determination. Thus a highly selective assay was proposed and applied to the determination of S2− in discharged water with the recovery of ca. 103%.  相似文献   

8.
A new, simple and accurate spectrofluorimetric method for the determination of metoclopramide hydrochloride was developed. The metoclopramide hydrochloride can remarkably enhance the luminescence intensity of the Tb3+ ion doped in PMMA matrix at λex = 360 nm in methanol at pH 6.9. The intensity of the emission band at 545 nm of Tb3+ ion doped in PMMA matrix is increased due to the energy transfer from metoclopramide hydrochloride to Tb3+ in the excited stated. The effect of different parameters, e.g., pH, temperature, Tb3+ concentration, foreign ions that control the fluorescence intensity of the produced ion associate was critically investigated. The calibration curve of the emission intensity at 545 nm shows linear response of metoclopramide over a concentration range of 5 × 10−5–5.0 × 10−8 M with detection limit of 8.7 × 10−10 M. The method was used successfully for the determination of metoclopramide in pharmaceutical preparations and human serum. The average recovery of 99.48% with standard deviation of 0.32% and 96.98% with standard deviation of 0.4%, of pharmaceutical preparations and human serum respectively, were obtained which compared will with the results obtained from standard LC method of average recovery 99.04% and standard deviation of 0.6% and average recovery of 98.19% with standard deviation of 0.6% of pharmaceutical preparations and human serum, respectively.  相似文献   

9.
A novel, simple, sensitive and selective spectrofluorimetric method was developed for the determination of trace amounts of chlorzoxazone and Ibuprofen in pharmaceutical tablets using optical sensor Eu-Tetracycline HCl doped in sol–gel matrix. The chlorzoxazone or Ibuprofen can remarkably enhance the luminescence intensity of Eu-Tetracycline HCl complex doped in a sol–gel matrix in dimethylformamide (DMF) at pH 9.7 and 6.3, respectively, λex = 400 nm. The enhancing of luminescence intensity peak of Eu-Tetracycline HCl complex at 617 nm is proportional to the concentration of chlorzoxazone or Ibuprofen a result that suggested profitable application as a simple optical sensor for chlorzoxazone or Ibuprofen assessment. The dynamic ranges found for the determination of chlorzoxazone and Ibuprofen concentration are 5 × 10−9–1 × 10−4 and 1 × 10−8–7 × 10−5 mol L−1, and the limit of detection (LOD) and quantitation limit of detection (LOQ) are 3.1 × 10−10 , 9.6 × 10−10 and 5.6 × 10−10, 1.7 × 10−9 mol L−1, respectively.  相似文献   

10.
This work describes the application of time resolved fluorescence in microtiterplates and electrochemical methods on glassy carbon electrode for investigating the interactions of europium-3-carboxycoumarin with pesticides aldicarb, methomyl and prometryne. Stern-volmer studies at different temperatures indicate that static quenching dominates for methomyl, aldicarb and prometryne. By using Lineweaver-Burk equation binding constants were determined at 303 K, 308 K and 313 K. A thermodynamic analysis showed that the reaction is spontaneous with ΔG being negative. The enthalpy ΔH and the entropy ΔS of reactions were all determined. A time-resolved (gated) luminescence-based method for determination of pesticides in microtiterplate format using the long-lived europium-3-carboxycoumarin has been developed. The limit of detection is 4.80, 5.06 and 8.01 μmol L−1 for methomyl, prometryne and aldicarb, respectively. This is the lowest limit of detection achieved so far for luminescent lanthanide-based probes for pesticides. The interaction of the probe with the pesticides has been investigated using cyclic voltammetry (CV), differential pulse polarography (DPP), square wave voltammetry (SWV) and linear sweep voltammetry (LSV) on a glassy carbon electrode in I = 0.1 mol L−1 p-toluenesulfonate at 25 °C. The diffusion coefficients of the reduced species are calculated. The main properties of the electrode reaction occurring in a finite diffusion space are the quasireversible maximum and the splitting of the net SWV peak for Eu(III) ions in the ternary complex formed . It was observed that the increase of the cathodic peak currents using LSV is linear with the increase of pesticides concentration in the range 5 × 10−7 to 1 × 10−5 mol L−1. The detection limit (DL) were about 1.01, 2.23 and 1.89 μmolL−1 for aldicarb, methomyl and prometryne, respectively. In order to assess the analytical applicability of the method, the influence of various potentially interfering species was examined. Influence of interfering species on the recovery of 10 μmol L−1 pesticides has been investigated.  相似文献   

11.
A sensitive time- resolved luminescence method for the determination of meloxicam (MX) in methanol and in aqueous solution is described. The method is based on the luminescence sensitization of europium (Eu3+) by formation of ternary complex with MX in the presence of 1,10- phenanthroline as coligand, Tween-80 as surfactant and gadolinium ion as a co-luminescence reagent. The signal for Eu- MX-1, 10- phenanthroline is monitored at λex = 360 nm and λem = 620 nm. Optimum conditions for the formation of the complex in aqueous system were 0.01 M TRIS buffer, pH 8.0, 1,10- phenanthroline (6.0 × 10−6 M) , Gd3+ (7.0 × 10−6 M), Tween-80 (0.28%) and 1.75 mM of Eu3+ which allows the determination of 20–800 ppb of MX with limit of detection (LOD) of 7 ppb. The relative standard deviations of the method range between 0.1 and 1.1% indicating excellent reproducibility of the method. The proposed method was successfully applied for the assay of MX in pharmaceutical formulations, plasma and in urine samples. Average recoveries of 99.8 ± 1.1%, 100.2 ± 0.9% and 100.9 ± 1.1% were obtained for MX in tablet, plasma and urine sample respectively.  相似文献   

12.
A novel and simple fluorescence enhancement method for selective pyrophosphate(PPi) sensing was proposed based on a 1:1 metal complex formation between bis(8-hydroxy quinoline-5-solphonat) chloride aluminum(III) (Al(QS)2Cl), (L) and PPi in aqueous solution. The linear response range covers a concentration range of 1.6 × 10−7 to 1.0 × 10−5 mol/L of PPi and the detection limit of 2.3 × 10−8 mol/L. The association constant of L-PPi complex was calculated 2.6 × 105 L/mol. L was found to show selectively and sensitively fluorescence enhancement toward PPi over than I3-, NO3-, CN, CO32−, Br, Cl, F, H2PO4 and SO42−, which was attributed to higher stability of inorganic complex between pyrophosphate and L.  相似文献   

13.
Zhang F  Wu X  Zhan J 《Journal of fluorescence》2011,21(5):1857-1864
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   

14.
The effect of temperature on the spectral luminescence characteristics of PbWO4:Tb3+ crystals with synchrotron and laser excitation is studied. If PbWO4:Tb3+ is excited by synchrotron radiation with λ = 88 nm at 300 K, a faint recombination luminescence of the impurity terbium is observed against the matrix luminescence. When the temperature is reduced to 8 K, the luminescence intensity of PbWO4:Tb3+ increases by roughly an order of magnitude and the characteristic luminescence of the unactivated crystal is observed. Excitation of PbWO4:Tb3+ by a nitrogen laser at 300 K leads to the appearance of emission from Tb3+ ions. At 90 K, a faint matrix luminescence is observed in addition to the activator emission. The formation of the luminescence excitation spectra for wavelengths of 60–320 nm is analyzed and the nature of the emission bands is discussed.  相似文献   

15.
It is found that silver nanoparticles (AgNPs) can further enhance the fluorescence intensity of curcumin (CU) - cetyltrimethylammonium bromide (CTAB) – nucleic acids and improve its anti-photobleaching activity. Under optimum conditions, the enhanced fluorescence intensity is proportion to the concentration of nucleic acids in the range of 2.0 × 10−8–1.0 × 10−6 g mL−1 for fish sperm DNA (fsDNA), 2.0 × 10−8–1.0 × 10−6 g mL−1 for calf thymus DNA (ctDNA), 1.0 × 10−8–1.0 × 10−6 g mL−1 for yeast RNA (yRNA), and their detection limits (S/N = 3) are 8.0 ng mL−1, 10.5 ng mL−1 and 5.8 ng mL−1, respectively. This method is used for determining the concentration of DNA in actual sample with satisfactory results. The interaction mechanism is also studied.  相似文献   

16.
The electrical characteristics of thin TiO2 films prepared by metal–organic chemical vapor deposition grown on a p-type InP substrate were studied. For a TiO2 film of 4.7 nm on InP without and with ammonium sulfide treatment, the leakage currents are 8.8×10−2 and 1.1×10−4 A/cm2 at +2 V bias and 1.6×10−1 and 8.3×10−4 A/cm2 at −2 V bias. The lower leakage currents of TiO2 with ammonium sulfide treatment arise from the improvement of interface quality. The dielectric constant and effective oxide charge number density are 33 and 2.5×1013 cm2, respectively. The lowest mid-gap interface state density is around 7.6×1011 cm−2 eV−1. The equivalent oxide thickness is 0.52 nm. The breakdown electric field increases with decreasing thickness in the range of 2.5 to 7.6 nm and reaches 9.3 MV/cm at 2.5 nm.  相似文献   

17.
In this study, a very sensitive and highly selective irreversible optical chemical sensor (optode) for mercury ions was described. The sensing scheme was based on the interaction of Hg (II) with a newly synthesized fluoroionophore; chloro phenyl imino propenyl aniline (CPIPA) in plasticized PVC membrane. The sensor membranes were tested for the determination of mercury ion in aqueous solutions by batch and flow-through methods. The optodes allow determination of Hg (II) in the working range of 1.0 × 10−9–1.0 × 10−5 M with a detection limit of 4.3 ppb. The sensor exhibited excellent selectivity for Hg (II) with respect to several common alkali, alkaline earth and transition metal ions. The association constant of the 1:1 complex formation for Hg (II) was found to be Ka = 1.86 × 105 M−1. The CPIPA exhibited high fluorescence quantum yield, long excitation and emission wavelength and high Stokes’ shift values in the solid matrix which makes it compatible with solid state optics.  相似文献   

18.
The complex of Tb(TPTZ)Cl3·3H2O was synthesized by adding the ethyl alcohol solution of TbCl3 (1 mmol) to the solution of 2,4,6-tris-(2-pyridyl)-s-triazine(TPTZ,1 mmol) with constant stirring. The solution which had been filtered was kept at the room temperature for 4 weeks, and then a kind of transparent crystal was formed. Besides, nine kinds of solid complexes in the different molar proportion of terbium to gadolinium had been synthesized by adopting the similar method mentioned above. It was inferred from the elemental analysis and rare earth complexometry that the composition of these complexes is (TbxGdy)(TPTZ)Cl3·3H2O (x : y = 0.9 : 0.1, 0.8 : 0.2, 0.7 : 0.3, 0.6 : 0.4, 0.5 : 0.5, 0.4 : 0.6, 0.3 : 0.7, 0.2 : 0.8, 0.1 : 0.9). The absorption spectra and photoluminescence of the complexes were determined in dimethylsulfoxide (DMF), which showed that the excitation of the complexes is mostly ligand based. The triplet state energy level of TPTZ was measured, indicating that the lowest excitation state energy level of Tb(III) and the triplet state energy level of TPTZ match well each other. The fluorescent data indicated that the fluorescent emission intensity of Tb3+ ions would be enhanced in the complexes after terbium was doped with Gd3+ ion. When x : y was 0.5 : 0.5, the fluorescent emission intensity was the largest. The result obtained by testing the X-ray diffraction of the monocrystal revealed that the molecular formula of the mono-crystal complex is [Tb(TPTZ)(H2O)6]Cl3·3H2O. The number of metal ion coordinates is nine, and the tridentate TPTZ and six water molecules are bonded with terbium respectively. Besides, it also revealed that the monocrystal belongs to the monoclinic system, and space group Cc with the following unit cell parameters is a = 1.4785 (3) nm, b = 1.0547 (2) nm, c = 1.7385 (4) nm, β = 94.42 (3)°, V = 2.7028 (9) nm3 and Z = 4.  相似文献   

19.
The fluorescence system of the norfloxacin-Tb3+- sodium dodecylbenzene sulfonate (SDBS) was investigated in this paper. The experiments indicated that the fluorescence intensity of the Tb3+-SDBS was greatly enhanced by the norfloxacin. On the basis of the above findings, a sensitive fluorimetric method for determining the norfloxacin was established. The fluorescence intensity was measured by a 1-cm quartz cell with the excitation wavelength of 290 nm and the emission wavelength of 545 nm. The enhanced fluorescence intensity of the system (Δ F) showed a good linear relationship with the concentration of norfloxacin in the range of 5.0×10−9 mol L−1–2.0×10−6 mol L−1, its correlation coefficient was 0.9991 and the detection limit (S/N=3) was 1.2×10−9 mol L−1. The presented method was used to determine the norfloxacin in real pharmaceutical samples. The luminescence mechanism was also discussed in detail. In the fluorescence system of the norfloxacin-Tb3+-SDBS, the SDBS not only acted as the surfactant, but also acted as the energy donor.  相似文献   

20.
A fluorimetric method based on fluorescence enhancement effect was developed for the determination of adenosine 5′-monophosphate (AMP) with 9-anthracene carboxylic acid (9-ANCA)–cetyl trimethyl ammonium bromide (CTAB) system. Fluorescence intensity of 9-ANCA was decreased by the addition of CTAB but addition of AMP again rose the intensity of 9-ANCA gradually. The observed fluorescence enhancement is attributed to the competitive binding reaction of 9-ANCA and adenosine to CTAB. The enhancement in the fluorescence intensity was found proportional to the concentration of AMP over the range 2.0 × 10−4 to 1.2 × 10−3 mol dm−3. The ion pair complex is formed spontaneously between 9-ANCA and CTAB. Since the binding interaction is larger for the adenosine–CTAB pair, the fluorophore 9-ANCA will be released. The quantum yield of free 9-ANCA is higher therefore its fluorescence observed at 417 nm wavelength is enhanced. This mechanism of competitive molecular interaction is further confirmed by conductometric measurements. The method was applied successfully for the determination of AMP from pharmaceutical sample. The method is more selective, sensitive and relatively free from interferences.  相似文献   

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