Simultaneous determination of microcystin contaminations in various vertebrates (fish, turtle, duck and water bird) from a large eutrophic Chinese lake, Lake Taihu, with toxic Microcystis blooms

This is the first to conduct Simultaneous determination of microcystin (MC) contaminations in multi-groups of vertebrates (fish, turtle, duck and water bird) from Lake Taihu with Microcystis blooms. MCs (-RR, -YR, -LR) in Microcystis scum was 328 mu g g(-1) DW. MCs reached 235 mu g g(-1) DW in intestinal contents of phytoplanktivorous silver carp, but never exceeded 0.1 mu g g(-1) DW in intestinal contents of other animals. The highest MC content in liver of fish was in Carassius auratus (150 ng g(-1) DW), followed by silver carp and Culter ilishaeformis, whereas the lowest was in common carp (3 ng g(-1) DW). In livers of turtle, duck and water bird, MC content ranged from 18 to 30 ng g(-1) DW. High MC level was found in the gonad, egg yolk and egg white of Nycticorax nycticorax and Anas platyrhynchos, suggesting the potential effect of MCs on water bird and duck embryos. High MC contents were identified for the first time in the spleens of N. nycticorax and A. platyrhynchos (6.850 and 9.462 ng g(-1) DW, respectively), indicating a different organotropism of MCs in birds. Lakes with deaths of turtles or water birds in the literatures had a considerably higher MC content in both cyanobacteria and wildlife than Lake Taihu, indicating that toxicity of cyanobacteria may determine accumulation level of MCs and consequently fates of aquatic wildlife. (C) 2009 Elsevier B.V. All rights reserved.

Simultaneous determination of microcystin-LR and its glutathione conjugate in fish tissues by liquid chromatography-tandem mass spectrometry

A sensitive and selective liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantitative determination of microcystin-LR (MC-LR) and its glutathione conjugate (MC-LR-GSH) in fish tissues. The analytes were extracted from fish liver and kidney using 0.01 M EDTA-Na-2-5% acetic acid, followed by a solid-phase extraction (SPE) on Oasis HLB and silica cartridges. High-performance liquid chromatography (HPLC) with electrospray ionization mass spectrometry, operating in selected reaction monitoring (SRM) mode, was used to quantify MC-LR and its glutathione conjugate in fish liver and kidney. Recoveries of analytes were assessed at three concentrations (0.2, 1.0, and 5 mu g g(-1) dry weight [DW]) and ranged from 91 to 103% for MC-LR, and from 65.0 to 75.7% for MC-LR-GSH. The assay was linear within the range from 0.02 to 5.0 mu g g(-1) DW, with a limit of quantification (LOQ) of 0.02 mu g g(-1) DW. The limit of detection (LOD) of the method was 0.007 mu g g(-1) DW in both fish liver and kidney. The overall precision was determined on three different days. The values for within- and between-day precision in liver and kidney were within 15%. This method was applied to the identification and quantification of MC-LR and its glutathione conjugate in liver and kidney of fish with acute exposure of MC-LR. (c) 2007 Elsevier B.V. All rights reserved.

Simultaneous determination of chromium(VI) and chromium(III) of bioavailable fraction in bottom mud by flow injection-atomic absorption spectroscopy

A rapid and sensitive method for separation and determination of Cr(VI) and Cr(III) in bottom mud of lake by flow injection on-line preconcentrtion system and GFAAS was developed. The available Cr(VI) and Cr(III) were extracted by HOAc or EDTA + NH4 NO3 and adsorbed simultaneously by an anion and a cation resin microclummn and then eluted simultaneously by 2 mol/L NH4 NO3 + 0.05 mol/L ascorbate and 2 mol/L H2SO4, respectively. The elution was performed for 50 s after adsorption for 2 min, and the efficiencies of elution were 85.4% - 94.8% and 96.7% - 106% for Cr(VI) and Cr(M) respectively. The detection limits of the method were 0.9 mu g/L and 2.7 mu g/L with relative standard deviations of 3.5% and 6.4% for the determination of Cr(VI) and Cr(III) in sample, respectively.

Simultaneous determination of methylene blue and new methylene blue by slab optical waveguide spectroscopy and artificial neural networks

A slab optical waveguide (SOWG) has been used for study of adsorption of both methylene blue (MB) and new methylene blue (NMB) in liquid-solid interface. Adsorption characteristics of MB and NMB on both bare SOWG and silanized SOWG by octadecyltrichlorosilane (ODS) were compared. The simultaneous determinations of both MB and NMB were explored by flow injection SOWG spectrophotometric analysis and artificial neural networks (ANNs) for the first time. Concentrations of MB and NMB were estimated simultaneously with the ANNs. Results obtained with SOWG were compared with those got by conventional UV-visible spectrophotometry. (C) 2003 Elsevier Science B.V All rights reserved.

Simultaneous determination of dopamine, ascorbic acid and uric acid with electrospun carbon nanofibers modified electrode

A novel carbon-nanofiber-modified carbon-paste electrode (CNF-CPE) was employed for the simultaneous determination of dopamine (DA), ascorbic acid (AA) and uric acid (UA) with good selectivity and high sensitivity. The CNFs were prepared by combination of electrospinning technique with thermal treatment method and were used without any pretreatment. In application to determination of DA, AA and UA in the ternary mixture, the pristine CNF-CPE exhibited well-separated differential pulse voltammetric peaks with high catalytic current. Low detection limits of 0.04 mu M, 2 mu M and 0.2 mu M for DA, AA and UA were obtained, with the linear calibration curves over the concentration range 0.04-5.6 mu M, 2-64 mu M and 0.8-16.8 mu M, respectively.

Simultaneous determination of pethidine and methadone by capillary electrophoresis with electrochemiluminescence detection of tris(2,2 '-bipyridyl)ruthenium(II)

In this paper, we described a simple and rapid method, capillary electrophoresis with electrochemiluminescence (CE-ECL) detection using tris(2,2'-bipyridyl)ruthenium(II) (Ru(bpy)(3)(2+)), to simultaneously detect pethidine and methadone. Analytes were injected to separation capillary of 67.5 cm length (25 mu m i.d., 360 mu m o.d.) by electrokinetic injection for 10 s at 10 kV.

Characterization of procaine metabolism as probe for the butyrylcholinesterase enzyme investigation by simultaneous determination of procaine and its metabolite using capillary electrophoresis with electrochemiluminescence detection

Capillary electrophoresis with electrochemiluminescene detection was used to characterize procaine hydrolysis as a probe for butyrylcholinesterase by in vitro procaine metabolism in plasma with butyrylcholinesterase acting as bioscavenger. Procaine and its metabolite N,N-diethylethanolamine were separated at 16 kV and then detected at 1.25 V in the presence of 5.0 mM Ru(bpy)(3)(2+), with the detection limits of 2.4 x 10(-7) and 2.0 x 10(-8) mol/L (S/N=3), respectively. The Michaelis constant K-m value was 1.73 x 10(-4) mol/L and the maximum velocity V-max was 1.62 x 10(-6) mol/L/min. Acetylcholine bromide and choline chloride presented inhibition effects on the enzymatic cleavage of procaine, with the 50% inhibition concentration (IC50) of 6.24 x 10(-3) and 2.94 x 10(-4) mol/L.

Simultaneous determination of dopamine and ascorbic acid at an in-site functionalized self-assembled monolayer on gold electrode

The in-site functionalization of 4-aminothiophenol (4-ATP) self-assembled monolayer on gold electrode at physiological pH yields a redox active monolayer of 4'-mercapto-N-phenylquinone diimine (MNPD). The functionalized electrode exhibits excellent electrocatalytic responses towards dopamine (DA) and ascorbic acid (AA), reducing the overpotentials by about 0.22 V and 0.34 V, respectively, with greatly enhanced current responses. Due to its different catalytic activities toward DA and AA, the modified electrode resolves the overlapping voltammetric responses of DA and AA into two well-defined voltammetric peaks by differential pulse voltammetry (DPV), which can be used for the simultaneous determination of these species in a mixture. The catalytic peak current obtained from DPV was linearly related to DA and AA concentration in the ranges of 5.0 x 10-6 - 1.25 x 10-4 M and 8.0 x 10-6 - 1.3 x 10-4 M with correlation coefficient of 0.999 and 0.998, respectively. The detective limits (3sigma) for DA and AA were found to be 1.2 x 10-6 M and 2.4 x 10-6 M, respectively.

Simultaneous determination of tramadol and lidocaine in urine by end-column capillary electrophoresis with electrochemiluminescence detection

Tramadol and lidocaine, used as analgesic and local anesthetic in surgery, are partly excreted by kidney. For the first time, we developed a simple and sensitive method, based on capillary electrophoresis with electrochemiluminescence (ECL) detection by end column mode without joint to monitor tramadol and lidocaine in urine. To eliminate the influence of ionic strength of urine sample, analytes were extracted by ether. Tripropylamine (TPA) was used as internal standard. ne recoveries of tramadol and lidocaine were between 94% and 97% at different levels. The method exhibited the linear range for the tramadol and lidocaine from 1.0 X 10(-7) to 1.0 X 10(-4) mol/L with correlation efficient of 0.998. The relative standard deviation (RSD) was 2.9% and 2.7% (n = 8) for tramadol and lidocaine, respectively. The limit of detection (LOD) was 6.0 x 10(-8) mol/L and 4.5 x 10(-8), mol/L (S/N = 3) for tramadol and lidocaine, respectively. The application for detecting tramadol and lidocaine in urine of patients showed that the method was valuable in clinical and biochemical laboratories for detecting tramadol, lidocaine and other tertiary amine pharmaceuticals for various purpose, such as metabolism investigation.

Simultaneous determination of 2-aminothiazole, 2-aminobenzothiazole and 2-mercaptobenzothiazole by capillary electrophoresis with end-column amperometric detection

Capillary electrophoresis with amperometric detection is evaluated for the simultaneous determination of 2-aminothiazole (A), 2-amino-benzothiazole (AB), 2-mercaptobenzothiazole (AM). The cyclic voltammogram, hydrodynamic voltammogram, effect of pH, concentration of buffer and separation voltage on the separation and the detection were studied. The conditions were optimized as follows: 50 mM phosphate buffet; pH 6.0, 2s at 17.5 kV sample injection, separation at 17.5 kV, 1.2 V as detection potential. The method provided low detection limit as 0.5 mu M, 0.05 mu M and 0.01 mu M, wide linear range 2-200 mu M, 10-200 mu M and 0.025-100 mu M for A, AB, and AM, respectively. The variations in peak current and migration time for 15 consecutive injections of a standard containing 5 mu M each compound were 3.7, 2.1, and 3.9%, and 1.2, 0.8, and 1.2%, for A, AB and AM, respectively. This method was employed to analyze river water.

Simultaneous determination of both the calibration constant in an electrochemical quartz crystal microbalance and the active surface area of a polycrystalline gold electrode

A novel method is employed for the simultaneous determination of both the calibration constant of an electrochemical quartz crystal microbalance (EQCM) and the active surface area of a polycrystalline gold electrode. A gold electrode: is immersed into a 1 mM KI/1 M H2SO4 solution and on which forms a neutral monolayer. The adsorbed iodine can then be completely oxidized into IO3-. The active surface area of a gold electrode can be obtained from the net electrolytic charge of the oxidation process, and the calibration constant in the EQCM can be calculated from the corresponding frequency shift. The result shows that this method is simple, convenient and valid. (C) 2000 Elsevier Science S.A. All rights reserved.

SIMULTANEOUS DETERMINATION OF GUANINE, URIC-ACID, HYPOXANTHINE AND XANTHINE IN HUMAN PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY WITH AMPEROMETRIC DETECTION

A reversed-phase high-performance liquid chromatographic method with amperometric detection is described for the separation and quantification of uric acid, guanine, hypoxanthine and xanthine. The isocratic separation of a standard mixture of the compounds was achieved in 5 min on a Spherisorb 5 C-18 reversed-phase column, with a mobile phase of NaH2PO4 (300 mmol dm(-3) pH 3.0)-methanol-acetonitrile-tetrahydrofuran (97.8 + 0.5 + 1.5 + 0.2). Uric acid, guanine, hypoxanthine and xanthine were completely separated, with detection limits in the range 2-20 pmol per injection. The effect of pH and the composition of the mobile phase on the separation are described. The hydrodynamic voltammograms of these compounds were recorded at a glassy carbon electrode. The linear range of the calibration graph for each compound was: uric acid; 1-5000 mu mol dm(-3); guanine, 0.5-2000 mu mol dm(-3); hypoxanthine, 0.1-500 mu mol dm(-3) and xanthine, 0.5-5000 mu mol dm(-3). The within- and between-day precision was good. The uric acid and hypoxanthine content in human plasma was measured using the proposed method. Good recoveries of uric acid (97.9-103%), hypoxanthine (98.0-99.2%), guanine (96.0-98.3%) and xanthine (96.0-102%) were obtained from human plasma. The results of electrochemical detection were in good agreement with those of UV detection.