Xilin Xiao

Synchronous fluorescence determination of urinary 1-hydroxypyrene, β-naphthol and 9-hydroxyphenanthrene based on the sensitizing effect of β-cyclodextrin

A novel method for the simultaneous determination of 1-hydroxypyrene (1-OHP), beta-naphthol (beta-NAP) and 9-hydroxyphenanthrene (9-OHPe) in human urine has been established by using synchronous fluorescence spectrometry. It was based on the fact that synchronous fluorescence spectrometry can resolve the broad-band overlapping of conventional fluorescence spectra, which arise from their similar molecular structures. Only one single scan is needed for quantitative determination of three compounds simultaneously when Deltalambda=15nm is chosen. The signals detected at these three wavelengths, 369.6, 330.0 and 358.0nm, vary linearly when the concentration of 1-OHP, beta-NAP and 9-OHPe is in the range of 2.16x10(-8)-1.50x10(-5)molL(-1), 1.20x10(-7)-1.10x10(-5)molL(-1) and 1.07x10(-7)-3.50x10(-5)molL(-1), respectively. The correlation coefficients for the standard calibration graphs were 0.994, 0.999 and 0.997 (n=7) for 1-OHP, beta-NAP and 9-OHPe, respectively. The limits of detection (LOD) for 1-OHP, beta-NAP and 9-OHPe were 6.47x10(-9)molL(-1), 3.60x10(-8)molL(-1) and 3.02x10(-8)molL(-1)with relative standard deviations (R.S.D.) of 4.70-6.40%, 2.80-4.20%, 3.10-4.90% (n=6), respectively. The method described here had been applied to determine traces of 1-OHP, beta-NAP and 9-OHPe in human urine, and the obtained results were in good agreement with those obtained by the HPLC method. In addition, the interaction modes between beta-cyclodextrin (beta-CD) and 1-OHP, beta-NAP or 9-OHPe, as well as the mechanism of the fluorescence enhancement were also discussed.

Double-receptor sandwich supramolecule sensing method for the determination of ATP based on uranyl-salophen complex and aptamer.

In this study, we report a double-receptor sandwich supramolecule sensing method for the determination of adenosine triphosphate (ATP). One receptor is a uranyl-salophen complex which can bind the triphosphate group in ATP selectively, and another is an anti-adenosine aptamer which is a single-stranded oligonucleotide and can recognize the adenosine group in ATP specifically. The uranyl-salophen complex was immobilized on the surface of amino-silica gel particles and used as the solid phase receptor of ATP. The anti-adenosine aptamer was labeled with a fluorescent group and used as the labeled receptor of ATP. In the procedure of ATP detection, ATP was first combined with the solid phase receptor and then conjugated with the labeled receptor to form a sandwich-type supramolecule. The conditions of fabricating solid phase receptor and the influence of manifold variables on the determination were studied. The experimental results demonstrate that the method has a number of advantages such as high selectivity, high sensitivity, good stability and low cost. Under optimal conditions, the linear range for detection of ATP is 0.2-5.0 nmol/mL with a detection limit of 0.037 nmol/mL. The proposed method was successfully applied for the determination of ATP in real samples with the recoveries of 96.8-103.3%.

Rapid simultaneous analysis of 1-hydroxypyrene, 2-hydroxyfluorene, 9-hydroxyphenanthrene, 1- and 2-naphthol in urine by first derivative synchronous fluorescence spectrometry using Tween-20 as a sensitizer.

A novel method of first derivative synchronous fluorescence was developed for the rapid simultaneous analysis of trace 1-hydroxypyrene (1-OHP), 1-naphthol (1-NAP), 2-naphthol (2-NAP), 9-hydroxyphenanthrene (9-OHPe) and 2-hydroxyfluorene (2-OHFlu) in human urine. Only one single scan was needed for quantitative determination of five compounds simultaneously when Deltalambda=10 nm was chosen. In the optimal experimental conditions, there was a linear relationship between the fluorescence intensity and the concentration of 1-OHP, 1-NAP, 2-NAP, 9-OHPe and 2-OHFlu in the range of 1.75 x 10(-9) to 4.50 x 10(-6) mol L(-1), 3.64 x 10(-8) to 2.20 x 10(-4) mol L(-1), 8.18 x 10(-9) to 1.20 x 10(-4) mol L(-1), 3.26 x 10(-9) to 8.50 x 10(-5) mol L(-1) and 4.88 x 10(-9) to 5.50 x 10(-6) mol L(-1), respectively. The limits of detection (LOD) were found to be 5.25 x 10(-10) mol L(-1) for 1-OHP, 1.10 x 10(-8) mol L(-1) for 1-NAP, 2.46 x 10(-9) mol L(-1) for 2-NAP, 9.77 x 10(-10) mol L(-1) for 9-OHPe and 1.46 x 10(-9) mol L(-1) for 2-OHFlu. The proposed method is reliable, selective and sensitive, and has been used successfully in the determination of traces of 1-OHP, 1-NAP, 2-NAP, 9-OHPe and 2-OHFlu in human urine samples, whose results were in good agreement with those gained by the HPLC method.

Resonance light scattering method for the determination of anionic surfactant with acridine orange

The resonance Rayleigh scattering (RRS), second-order scattering (SOS) and frequency-double scattering (FDS) spectra of sodium dodecylbenzene sulfonate (SDBS) (anionic surfactant (AS)) with acridine orange (AO) system were studied. Experimental results showed that when lambda(em) = lambda(ex) = 537 nm, the RRS peak of AO was greatly enhanced with the increase of SDBS concentration at a pH range of 1.8-4.0. The linear range of the calibration curve for SDBS was 0.028-8.71 mg L(-1) with a detection limit of 8.36 microg L(-1) when the AO concentration was 2.5 x 10(-5)mol L(-1). The method has been applied to the determination of trace amount of AS in environmental water samples with satisfactory results. In addition, when lambda(em) = 321 nm and lambda(ex) = 642 nm, the intensity of FDS was proportional to the SDBS concentration ranging from 0.014 to 8.71 mg L(-1) and the correlation coefficient was 0.993 with a detection limit of 4.31 microg L(-1); when lambda(em) = 642 nm and lambda(ex) = 321 nm, the intensity of SOS was proportional to the SDBS concentration ranging from 0.050 to 8.71 mg L(-1), and the correlation coefficient was 0.993 with a detection limit of 14.9 microg L(-1).

Separation and determination of trace uranium using a double-receptor sandwich supramolecule method based on immobilized salophen and fluorescence labeled oligonucleotide

A double-receptor sandwich supramolecule method for the separation and determination of trace uranium was proposed in this paper. One receptor is a salophen which can react with uranyl to form a uranyl-salophen complex, and another receptor is an oligonucleotide which can bind uranyl to form oligonucleotide-uranyl-salophen supramolecule. The salophen was immobilized on the surface of silica gel particles and used as the solid phase receptor for separating uranium from solution. The oligonucleotide was labeled with a fluorescent group and used as the labeled receptor for quantitatively analyzing uranium. In the procedure of separation and determination, uranyl ion was first combined with the solid phase receptor and then conjugated with the labeled receptor to form the sandwich-type supramolecule. The labeled receptor in the sandwich supramolecule was then eluted and determined by fluorescence analysis. The experimental results demonstrate that this method has a number of advantages such as high selectivity, excellent pre-concentration capability, high sensitivity, good stability and low cost. Under optimal conditions, the linear range for the detection of uranium is 0.5-30.0 ng mL(-1) with a detection limit of 0.2 ng mL(-1). The proposed method was successfully applied for the separation and determination of uranium in real samples with the recoveries of 95.0-105.5%.

Spectroscopic study on the reactions of bis-salophen with uranyl and then with fructose 1,6-bisphosphate and the analytical application

The chelating reaction of bis-salophen with uranyl to form binuclear complex uranyl-bis-salophen (UBS) was studied by fluorescence spectroscopy. The coordination reaction of UBS with fructose 1,6-bisphosphate (F-1,6-BP) to form supramolecular polymer was then studied by resonance light scattering (RLS) spectroscopy. The reaction of bis-salophen with uranyl results in a remarkable enhancement of fluorescence intensity. The maximum emission wavelength of the fluorescence is at 471nm. The reaction of UBS with F-1,6-BP results in a remarkable enhancement of RLS intensity. The maximum scattering wavelength of the RLS is at 460nm. The two reactions were used to establish fluorescence method for the determination of uranium (VI) and RLS method for the determination of F-1,6-BP, respectively. Under optimum conditions, the linear ranges for the detection of uranium (VI) and F-1,6-BP are 0.003-0.35nmol/mL and 0.05-5.0nmol/mL, respectively. The detection limits are 0.0017nmol/mL and 0.020nmol/mL, respectively. The proposed fluorescence method has been successfully applied for the determination of uranium (VI) in environmental water samples with the recoveries of 97.0-104.0%. The proposed RLS method has also been successfully applied for the determination of F-1,6-BP in medicine injection samples with the recoveries of 98.5-102.3%.

Study on the interaction among pyronine Y, potassium bromate and naphthols by absorption, three-dimension fluorescence and resonance light scattering spectra and their application

A novel method for the determination of trace naphthols was proposed based on naphthols, potassium bromate and pyronine Y in dilute sulfuric acid medium can react to form ion-association complexes, which not only resulted in the changes of the three-dimension fluorescence spectra, absorption spectra and the quenching of fluorescence, but also resulted in the great enhancement of resonance light scattering (RLS). The characteristics of RLS spectra, the effective factors and optimum conditions of reaction were studied. It was found that the enhanced intensity of RLS at 396 nm was proportional to the concentration of 1-naphthol and 2-naphthol in the range of 41.4 approximately 3024 ng mL(-1) and 38.3 approximately 3068 ng mL(-1), respectively. The urine samples analysis of the relative standard deviation was 3.1-7.1% and the average recovery was 96.0% (n=6). The present method had been applied to the determination of trace naphthols in human urine, the obtained results were in good agreement with those obtained by the HPLC method; moreover, we had carried on an initial study of the reaction mechanism in terms of spectral characteristics.

Determination of fructose 1,6-bisphosphate using a double-receptor sandwich type fluorescence sensing method based on uranyl–salophen complexes

In this paper, we report a double-receptor sandwich type fluorescence sensing method for the determination of fructose bisphosphates (FBPs) using fructose 1,6-bisphosphate (F-1,6-BP) as a model analyte based on uranyl-salophen complexes. The solid phase receptor is an immobilized uranyl-salophen (IUS) complex which is bound on the surface of glass slides by covalent bonds. The labeled receptor is another uranyl-salophen complex containing a fluorescence group, or uranyl-salophen-fluorescein (USF). In the procedure of determining F-1,6-BP in sample solution, F-1,6-BP is first adsorbed on the surface of the glass slide through the coordination reaction of F-1,6-BP with IUS. It then binds USF through another coordination reaction to form a sandwich-type structure of IUS-F-1,6-BP-USF. The amount of F-1,6-BP is detected by the determination of the fluorescence intensity of IUS-F-1,6-BP-USF bound on the glass slide. Under optimal conditions, the linear range for the detection of F-1,6-BP is 0.05-5.0 nmol mL(-1) with a detection limit of 0.027 nmol mL(-1). The proposed method has been successfully applied for the determination of F-1,6-BP in real samples with satisfactory results.

Determination of trace formaldehyde in blood plasma by resonance fluorescence technology.

A novel method for the determination of trace formaldehyde in blood plasma has been established by using resonance fluorimetry technique. It was based on the fact that oxidation of pyronine Y by potassium bromate was catalyzed by formaldehyde in sulfuric acid. When the wavelength interval was at Δλ=0 nm, it was found that the decreased intensity (ΔF) of resonance fluorescence at 574.6 nm was proportional to the concentration of formaldehyde in the range of 1.27×10(-2) to 2.28 μg mL(-1). The limit of detection and the average recovery for formaldehyde were 3.80 ng mL(-1) and 101.6% (n=6), respectively. The present method had been applied to the determination of trace formaldehyde in blood plasma, and the obtained results were in good agreement with those obtained by the resonance light scattering method.

A highly sensitive and selective sensor based on a graphene-coated carbon paste electrode modified with a computationally designed boron-embedded duplex molecularly imprinted hybrid membrane for the sensing of lamotrigine

An innovative electrochemical sensor, based on a carbon paste electrode (CPE) modified with graphene (GR) and a boron-embedded duplex molecularly imprinted hybrid membrane (B-DMIHM), was fabricated for the highly sensitive and selective determination of lamotrigine (LMT). Density functional theory (DFT) was employed to study the interactions between the template and monomers to screen appropriate functional monomers for rational design of the B-DMIHM. The distinct synergic effect of GR and B-DMIHM was evidenced by the positive shift of the reduction peak potential of LMT at B-DMIHM/GR modified CPE (B-DMIHM/GR/CPE) by about 300mV, and the 13-fold amplification of the peak current, compared to a bare carbon paste electrode (CPE). The electrochemical reduction mechanism of lamotrigine was investigated by different voltammetric techniques. It was illustrated that square wave voltammetry (SWV) was more sensitive than different pulse voltammetry (DPV) for the quantitative analysis of LMT. Thereafter, a highly sensitive electroanalytical method for LMT was established by SWV at B-DMIHM/GR/CPE with a good linear relationship from 5.0×10-8 to 5.0×10-5 and 5.0×10-5 to 3.0×10-4molL-1 with a lower detection limit (1.52×10-9molL-1) based on the lower linear range(S/N=3). The practical application of the sensor was demonstrated by determining the concentration of LMT in pharmaceutical and biological samples with good precision (RSD 1.04-4.41%) and acceptable recoveries (92.40-107.0%).