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Sample records for nanotube-enhanced flow-injection amperometric

  1. A novel stopped flow injection-amperometric procedure for the determination of chlorate.

    Science.gov (United States)

    Tue-Ngeun, Orawan; Jakmunee, Jaroon; Grudpan, Kate

    2005-12-15

    A novel stopped flow injection-amperometric (sFI-Amp) procedure for determination of chlorate has been developed. The reaction of chlorate with excess potassium iodide and hydrochloric acid, forming iodine/triiodide that is further electrochemically reduced at a glassy carbon electrode at +200mV versus Ag/AgCl electrode is employed. In order to increase sensitivity without using of too high acid concentration, promoting of the reaction by increasing reaction time and temperature can be carried out. This can be done without increase of dispersion of the product zone by stopping the flow while the injected zone is being in a mixing coil which is immersed in a water bath of 55+/-0.5 degrees C. In a closed system of FIA, a side reaction of oxygen with iodide is also minimized. Under a set of conditions, linear calibration graphs were in the ranges of 1.2x10(-6)-6.0x10(-5)moll(-1)and 6.0x10(-5)-6.0x10(-4)moll(-1). A sample throughput of 25h(-1) was accomplished. Relative standard deviation was 2% (n=21, 1.2x10(-4)moll(-1) chlorate). The proposed sFI-Amp procedure was successfully applied to the determination of chlorate in soil samples from longan plantation area.

  2. Flow injection analysis using carbon film resistor electrodes for amperometric determination of ambroxol.

    Science.gov (United States)

    Felix, Fabiana S; Brett, Christopher M A; Angnes, Lúcio

    2008-06-30

    Flow injection analysis (FIA) using a carbon film sensor for amperometric detection was explored for ambroxol analysis in pharmaceutical formulations. The specially designed flow cell designed in the lab generated sharp and reproducible current peaks, with a wide linear dynamic range from 5x10(-7) to 3.5x10(-4) mol L(-1), in 0.1 mol L(-1) sulfuric acid electrolyte, as well as high sensitivity, 0.110 Amol(-1) L cm(-2) at the optimized flow rate. A detection limit of 7.6x10(-8) mol L(-1) and a sampling frequency of 50 determinations per hour were achieved, employing injected volumes of 100 microL and a flow rate of 2.0 mL min(-1). The repeatability, expressed as R.S.D. for successive and alternated injections of 6.0x10(-6) and 6.0x10(-5) mol L(-1) ambroxol solutions, was 3.0 and 1.5%, respectively, without any noticeable memory effect between injections. The proposed method was applied to the analysis of ambroxol in pharmaceutical samples and the results obtained were compared with UV spectrophotometric and acid-base titrimetric methods. Good agreement between the results utilizing the three methods and the labeled values was achieved, corroborating the good performance of the proposed electrochemical methodology for ambroxol analysis.

  3. Development of flow injection method for indirect copper determination with amperometric detection in drinking water samples

    Directory of Open Access Journals (Sweden)

    Nikolić-Mandić Snežana

    2012-01-01

    Full Text Available A gas-diffusion flow injection method with amperometric detection for indirect copper determination on a silver electrode is developed. The flow through system is equipped with two injection valves and a gas-diffusion unit. In the first step, a signal of cyanide solution was recorded. In the following step a signal of cyanide in the presence of copper was measured. Interferences (Cd(II, Co(II, Ag(I, Ni(II, Fe(III, Hg(II and Zn(II were investigated and successfully removed. The calibration graph is linear in the range 1-90 μmol dm-3 of copper, correlation coefficient is 0.993, the regression equation is I = (0.0455±0.0015c + (0.4611±0.0671, I is relative signal decrease in μA and c is concentration in μmol dm-3. Relative standard deviation for six consecutive injections of 30 μmol dm-3 copper(II was 1.47 % and for 1 μmol dm-3 copper(II was 3.40 %. The detection limit, calculated as 3 s/m (where s is a standard deviation of nine measurement of a reagent blank and m is the slope of the calibration curve, was 0.32 μmol dm-3, which corresponds to 2.44 ng of copper(II (loop volume was 0.12 cm3. The method enables 60 analyses per hour and it was successfully applied on determination of copper in drinking water samples. [Acknowledgements. The authors acknowledge the grant from the Ministry of Education and Science of the Republic of Serbia, Project number 172051

  4. Polarographic study of acrolein and its determination by flow injection with amperometric detection at a mercury electrode.

    Science.gov (United States)

    Naranjo Rodríguez, I; Muñoz Leyva, J A; Hidalgo Hidalgo de Cisneros, J L

    1996-07-01

    A study of the electrochemical behavior of acrolein at a dropping mercury electrode using different polarographic techniques is described. Theoretical studies of the reversibility of the wave of acrolein were carried out using two different polarographic techniques: direct current tast and differential pulse. Differential pulse polarography may be used to determine acrolein concentration in a Britton-Robinson buffer solution of pH 10 in the ranges 2 x 10(-7)10(-8) and 5 x 10(-8)-10(-4) mol dm(-3) and a coefficient of variation of 1.7% for a concentration of 10(-5)mol dm(-3). A flow injection method with amperometric detection at a potential of -1.4V using a mercury electrode is also described. Before each injection, any drop hanging from the tip of the capillary needs to be dislodged and a new electrode drop dispensed; three different drop sizes were tested. A linear relationship between peak intensity and acrolein concentration was obtained in the range 10(-5)-10(-7) mol dm(-3), with a detection limit of 9.8 x 10(-8) mol dm(-) 3 and a coefficient of variation of 2.9% for a 2 x 10(-7) mol dm(-3) concentration. Several organic and inorganic species were tested in order to ascertain whether they interfered with the signal for acrolein. The proposed methods were applied to the determination of acrolein in seawater samples.

  5. Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

    Science.gov (United States)

    Jakmunee, Jaroon; Junsomboon, Jaroon

    2009-09-15

    A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

  6. Simple flow injection for determination of sulfite by amperometric detection using glassy carbon electrode modified with carbon nanotubes-PDDA-gold nanoparticles.

    Science.gov (United States)

    Amatatongchai, Maliwan; Sroysee, Wongduan; Chairam, Sanoe; Nacapricha, Duangjai

    2015-02-01

    A new approach is presented for sensitive and selective measurement of sulfite (SO3(2-)) in beverages based on a simple flow injection system with amperometric detection. In this work, the sulfite sensor was a glassy carbon electrode modified with multiwall carbon nanotubes-poly(diallyldimethylammonium chloride)-gold nanoparticles composites (CNTs-PDDA-AuNPs/GC). Electrochemical oxidation of sulfite with this electrode was first studied in 0.1M phosphate buffer (pH 7.0) using cyclic voltammetry. The results indicated that the CNTs-PDDA-AuNPs/GC electrode possesses electrocatalytic activity for the oxidation of sulfite with high sensitivity and selectivity. Sulfite was quantified using amperometric measurement with the new sensor at +0.4V vs Ag/AgCl in conjunction with flow injection. The linear working range for the quantitation of sulfite was 2-200 mg L(-1) (r(2)=0.998) with a detection limit of 0.03 mg L(-1) (3σ of blank) and an estimated precision of 1.5%.The proposed method was successfully applied to the determination of sulfite in fruit juices and wines with a sample throughput of 23 samples per hour. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Flow-Injection Amperometric Determination of Tacrine based on Ion Transfer across a Water–Plasticized Polymeric Membrane Interface

    Directory of Open Access Journals (Sweden)

    C. Rueda

    2007-07-01

    Full Text Available A flow-injection pulse amperometric method for determining tacrine, based onion transfer across a plasticized poly(vinyl chloride (PVC membrane, was developed. Afour-electrode potentiostat with ohmic drop compensation was used, while a flow-throughcell incorporated the four electrodes and the membrane, which containedtetrabutylammonium tetraphenylborate. The influence of the applied potential and of theflow-injection variables on the determination of tacrine was studied. In the selectedconditions, a linear relationship between peak height and tacrine concentration was foundup to 4x10-5M tacrine. The detection limit was 1x10-7M. Good repeatability was obtained.Some common ions and pharmaceutical excipients did not interfere.

  8. Flow injection determination of choline in milk hydrolysates by an immobilized enzyme reactor coupled to a selective hydrogen peroxide amperometric sensor

    Energy Technology Data Exchange (ETDEWEB)

    Pati, Sandra [Dipartimento di Chimica, Universita degli Studi di Bari, Via Orabona 4, 70126 Bari (Italy); Quinto, Maurizio [Dipartimento di Scienze Agroambientali, Chimica e Difesa Vegetale, Universita degli Studi di Foggia, Via Napoli 25, 71100 Foggia (Italy); Palmisano, Francesco [Dipartimento di Chimica, Universita degli Studi di Bari, Via Orabona 4, 70126 Bari (Italy)]. E-mail: palmisano@chimica.uniba.it

    2007-07-02

    A choline oxidase (ChO) immobilized enzyme reactor (IMER) prepared by glutaraldehyde coupling of the enzyme on aminopropyl modified controlled pore glass beads is described. The ChO-IMER was coupled, in a flow injection configuration system, to an interference free hydrogen peroxide amperometric sensor based on a Pt surface modified by an overoxidized polypyrrole film. The resulting analytical device responds selectively to choline and displays a sensitivity of 46.9 {+-} 0.2 {mu}C mM{sup -1} and a limit of detection, calculated at a signal-to-noise ratio equal to 3, of 7 {mu}M. Sensitivity remains constant for about 20 days and then starts to slowly deteriorate and after 2 months a 70% of the initial sensitivity was still retained. The application to choline determination in milk hydrolysates is demonstrated. Short- and long-term drift observed in the analytical response can be corrected by a bracketing technique.

  9. Flow-injection amperometric determination of glucose using a biosensor based on immobilization of glucose oxidase onto Au seeds decorated on core Fe₃O₄ nanoparticles.

    Science.gov (United States)

    Samphao, Anchalee; Butmee, Preeyanut; Jitcharoen, Juthamas; Švorc, Ľubomír; Raber, Georg; Kalcher, Kurt

    2015-09-01

    An amperometric biosensor based on chemisorption of glucose oxidase (GOx) on Au seeds decorated on magnetic core Fe3O4 nanoparticles (Fe3O4@Au) and their immobilization on screen-printed carbon electrode bulk-modified with manganese oxide (SPCE{MnO2}) was designed for the determination of glucose. The Fe3O4@Au/GOx modified SPCE{MnO2} was used in a flow-injection analysis (FIA) arrangement. The experimental conditions were investigated in amperometric mode with the following optimized parameters: flow rate 1.7 mL min(-1), applied potential +0.38 V, phosphate buffer solution (PBS; 0.1 mol L(-1), pH 7.0) as carrier and 3.89 unit mm(-2) enzyme glucose oxidase loading on the active surface of the SPCE. The designed biosensor in FIA arrangement yielded a linear dynamic range for glucose from 0.2 to 9.0 mmol L(-1) with a sensitivity of 2.52 µA mM(-1) cm(-2), a detection limit of 0.1 mmol L(-1) and a quantification limit of 0.3 mmol L(-1). Moreover, a good repeatability of 2.8% (number of measurements n=10) and a sufficient reproducibility of 4.0% (number of sensors n=3) were achieved. It was found that the studied system Fe3O4@Au facilitated not only a simpler enzyme immobilization but also provided wider linear range. The practical application of the proposed biosensor for FIA quantification of glucose was tested in glucose sirup samples, honeys and energy drinks with the results in good accordance with those obtained by an optical glucose meter and with the contents declared by the producers. Copyright © 2015. Published by Elsevier B.V.

  10. Fabrication of an Amperometric Flow-Injection Microfluidic Biosensor Based on Laccase for In Situ Determination of Phenolic Compounds

    Directory of Open Access Journals (Sweden)

    Juan C. Gonzalez-Rivera

    2015-01-01

    Full Text Available We aim to develop an in situ microfluidic biosensor based on laccase from Trametes pubescens with flow-injection and amperometry as the transducer method. The enzyme was directly immobilized by potential step chronoamperometry, and the immobilization was studied using cyclic voltammetry and electrochemical impedance spectroscopy. The electrode response by amperometry was probed using ABTS and syringaldazine. A shift of interfacial electron transfer resistance and the electron transfer rate constant from 18.1 kΩ to 3.9 MΩ and 4.6 × 10−2 cm s−1 to 2.1 × 10−4 cm s−1, respectively, evidenced that laccase was immobilized on the electrode by the proposed method. We established the optimum operating conditions of temperature (55°C, pH (4.5, injection flow rate (200 µL min−1, and applied potential (0.4 V. Finally, the microfluidic biosensor showed better lower limit of detection (0.149 µM and sensitivity (0.2341 nA µM−1 for ABTS than previous laccase-based biosensors and the in situ operation capacity.

  11. Cost-effective flow injection amperometric system with metal nanoparticle loaded carbon nanotube modified screen printed carbon electrode for sensitive determination of hydrogen peroxide.

    Science.gov (United States)

    Reanpang, Preeyaporn; Themsirimongkon, Suwaphid; Saipanya, Surin; Chailapakul, Orawon; Jakmunee, Jaroon

    2015-11-01

    Various metal nanoparticles (NPs) decorated on carbon nanotube (CNT) was modified on the home-made screen printed carbon electrode (SPCE) in order to enhances sensitivity of hydrogen peroxide (H2O2) determination. The simple casting method was used for the electrode modification. The monometallic and bimetallic NPs modified electrodes were investigated for their electrochemical properties for H2O2 reduction. The Pd-CNT/SPCE is appropriated to measure the H2O2 reduction at a potential of -0.3 V, then this modified electrode was incorporated with a home-made flow through cell and applied in a simple flow injection amperometry (FI-Amp). Some parameters influencing the resulted modified electrode and the FI-Amp system were studied. The proposed detection system was able to detect H2O2 in the range of 0.1-1.0 mM, with detection limit of 20 µM. Relative standard deviation for 100 replicated injections of 0.6 mM H2O2 was 2.3%. The reproducibility of 6 electrodes preparing in 3 different lots was 8.2%. It was demonstrated for determination of H2O2 in disinfectant, hair colorant and milk samples. Recoveries in the range of 90-109% were observed. The developed system provided high stability, good repeatability, high sample throughput and low reagent consumption. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Modified and reverse radiometric flow injection analysis

    Energy Technology Data Exchange (ETDEWEB)

    Myint, U; Ba, H; Khin, M M; Aung, K; Thida, [Yangon Univ. (Myanmar). Dept. of Chemistry; Toelgyessy, J [Slovak Technical Univ., Bratislava (Slovakia). Dept. of Environmental Science

    1994-06-01

    Determination of [sup 137]Cs and [sup 60]Co by using modified and reverse radiometric flow injection analysis is described. Two component RFIA was also realized using [sup 60]Co and [sup 137]Cs radionuclides. (author) 2 refs.; 5 figs.

  13. Flow Injection Analysis in Industrial Biotechnology

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2009-01-01

    Flow injection analysis (FIA) is an analytical chemical continuous-flow (CF) method which in contrast to traditional CF-procedures does not rely on complete physical mixing (homogenisation) of the sample and the reagent(s) or on attaining chemical equilibria of the chemical reactions involved. Ex...

  14. Retro-review of flow injection analysis

    DEFF Research Database (Denmark)

    Ruzicka, Jaromir; Hansen, Elo Harald

    2008-01-01

    It is indeed unusual for authors to review their own monograph – J. Ruzicka, E.H. Hansen, Flow Injection Analysis, 2nd Edition, Wiley, Chichester, West Sussex, UK, 1988. – and even more so if the book was published 20 years ago. Yet such an exercise might yield a perspective on the progress of an...

  15. Radiometric flow injection analysis with an ASIA (Ismatec) analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Myint, U; Win, N; San, K; Han, B; Myoe, K M [Yangon Univ. (Myanmar). Dept. of Chemistry; Toelgyessy, J [Slovak Technical Univ., Bratislava (Slovakia). Dept. of Environmental Science

    1994-07-01

    Radiometric Flow Injection Analysis of a radioactive ([sup 131]I) sample is described. For analysis an ASIA (Ismatec) analyzer with a NaI(Tl) scintillation detector was used. (author) 5 refs.; 3 figs.

  16. Implantable enzyme amperometric biosensors.

    Science.gov (United States)

    Kotanen, Christian N; Moussy, Francis Gabriel; Carrara, Sandro; Guiseppi-Elie, Anthony

    2012-05-15

    The implantable enzyme amperometric biosensor continues as the dominant in vivo format for the detection, monitoring and reporting of biochemical analytes related to a wide range of pathologies. Widely used in animal studies, there is increasing emphasis on their use in diabetes care and management, the management of trauma-associated hemorrhage and in critical care monitoring by intensivists in the ICU. These frontier opportunities demand continuous indwelling performance for up to several years, well in excess of the currently approved seven days. This review outlines the many challenges to successful deployment of chronically implantable amperometric enzyme biosensors and emphasizes the emerging technological approaches in their continued development. The foreign body response plays a prominent role in implantable biotransducer failure. Topics considering the approaches to mitigate the inflammatory response, use of biomimetic chemistries, nanostructured topographies, drug eluting constructs, and tissue-to-device interface modulus matching are reviewed. Similarly, factors that influence biotransducer performance such as enzyme stability, substrate interference, mediator selection and calibration are reviewed. For the biosensor system, the opportunities and challenges of integration, guided by footprint requirements, the limitations of mixed signal electronics, and power requirements, has produced three systems approaches. The potential is great. However, integration along the multiple length scales needed to address fundamental issues and integration across the diverse disciplines needed to achieve success of these highly integrated systems, continues to be a challenge in the development and deployment of implantable amperometric enzyme biosensor systems. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. AAO-CNTs electrode on microfluidic flow injection system for rapid iodide sensing.

    Science.gov (United States)

    Phokharatkul, Ditsayut; Karuwan, Chanpen; Lomas, Tanom; Nacapricha, Duangjai; Wisitsoraat, Anurat; Tuantranont, Adisorn

    2011-06-15

    In this work, carbon nanotubes (CNTs) nanoarrays in anodized aluminum oxide (AAO-CNTs) nanopore is integrated on a microfluidic flow injection system for in-channel electrochemical detection of iodide. The device was fabricated from PDMS (polydimethylsiloxane) microchannel bonded on glass substrates that contains three-electrode electrochemical system, including AAO-CNTs as a working electrode, silver as a reference electrode and platinum as an auxiliary electrode. Aluminum, stainless steel catalyst, silver and platinum layers were sputtered on the glass substrate through shadow masks. Aluminum layer was then anodized by two-step anodization process to form nanopore template. CNTs were then grown in AAO template by thermal chemical vapor deposition. The amperometric detection of iodide was performed in 500-μm-wide and 100-μm-deep microchannels on the microfluidic chip. The influences of flow rate, injection volume and detection potential on the current response were optimized. From experimental results, AAO-CNTs electrode on chip offers higher sensitivity and wider dynamic range than CNTs electrode with no AAO template. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

    The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

  19. Electrochemical study and flow injection analysis of paracetamol in pharmaceutical formulations based on screen-printed electrodes and carbon nanotubes

    International Nuclear Information System (INIS)

    Fanjul-Bolado, Pablo; Lamas-Ardisana, Pedro Jose; Hernandez-Santos, David; Costa-Garcia, Agustin

    2009-01-01

    Acetaminophenol or paracetamol is one of the most commonly used analgesics in pharmaceutical formulations. Acetaminophen is electroactive and voltammetric mechanistic studies for the electrode processes of the acetaminophenol/N-acetyl-p-quinoneimine redox system are presented. Carbon nanotubes modified screen-printed electrodes with enhanced electron transfer properties are used for the study of the electrochemical-chemical oxidation mechanism of paracetamol at pH 2.0. Quantitative analysis of paracetamol by using its oxidation process (in a Britton-Robinson buffer solution pH 10.0) at +0.20 V (vs. an Ag pseudoreference electrode) on an untreated screen-printed carbon electrode (SPCE) was carried out. Thus, a cyclic voltammetric based reproducible determination of acetaminophen (R.S.D., 2.2%) in the range 2.5 x 10 -6 M to 1 x 10 -3 M, was obtained. However, when SPCEs are used as amperometric detectors coupled to a flow injection analysis (FIA) system, the detection limit achieved for paracetamol was 1 x 10 -7 M, one order of magnitude lower than that obtained by voltammetric analysis. The repeatability of the amperometric detection with the same SPCE is 2% for 15 successive injections of 10 -5 M acetaminophen and do not present any memory effect. Finally, the applicability of using screen-printed carbon electrodes for the electrochemical detection of paracetamol (i.e. for quality control analysis) was demonstrated by using two commercial pharmaceutical products.

  20. Electrochemical study and flow injection analysis of paracetamol in pharmaceutical formulations based on screen-printed electrodes and carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Fanjul-Bolado, Pablo [DropSens, S.L., Edificio Severo Ochoa, Campus El Cristo, 33006 Oviedo, Asturias (Spain); Lamas-Ardisana, Pedro Jose [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, Julian Claveria 8, 33006 Oviedo, Asturias (Spain); Hernandez-Santos, David [DropSens, S.L., Edificio Severo Ochoa, Campus El Cristo, 33006 Oviedo, Asturias (Spain); Costa-Garcia, Agustin, E-mail: costa@fq.uniovi.es [Departamento de Quimica Fisica y Analitica, Universidad de Oviedo, Julian Claveria 8, 33006 Oviedo, Asturias (Spain)

    2009-04-13

    Acetaminophenol or paracetamol is one of the most commonly used analgesics in pharmaceutical formulations. Acetaminophen is electroactive and voltammetric mechanistic studies for the electrode processes of the acetaminophenol/N-acetyl-p-quinoneimine redox system are presented. Carbon nanotubes modified screen-printed electrodes with enhanced electron transfer properties are used for the study of the electrochemical-chemical oxidation mechanism of paracetamol at pH 2.0. Quantitative analysis of paracetamol by using its oxidation process (in a Britton-Robinson buffer solution pH 10.0) at +0.20 V (vs. an Ag pseudoreference electrode) on an untreated screen-printed carbon electrode (SPCE) was carried out. Thus, a cyclic voltammetric based reproducible determination of acetaminophen (R.S.D., 2.2%) in the range 2.5 x 10{sup -6} M to 1 x 10{sup -3} M, was obtained. However, when SPCEs are used as amperometric detectors coupled to a flow injection analysis (FIA) system, the detection limit achieved for paracetamol was 1 x 10{sup -7} M, one order of magnitude lower than that obtained by voltammetric analysis. The repeatability of the amperometric detection with the same SPCE is 2% for 15 successive injections of 10{sup -5} M acetaminophen and do not present any memory effect. Finally, the applicability of using screen-printed carbon electrodes for the electrochemical detection of paracetamol (i.e. for quality control analysis) was demonstrated by using two commercial pharmaceutical products.

  1. Flow Injection Analysis: A Revolution in Modern Analytical Chemistry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    A review is made of the fundamentals of Flow Injection Analysis (FIA), and the versatility and applicability of this analytical concept is demonstrated by a series of examples, comprizing the use of different types of FIA-manifolds and various detection devices (optical and electrochemical...

  2. Spectrofluorimetric determination of cerium by flow injection analysis

    International Nuclear Information System (INIS)

    Liu Shaorong; Meng Jian; Liu Wenhua

    1990-01-01

    A spectrofluorimetric method for the determination of cerium (λ ex/em:251/365 nm) in hydrochloric acid solution by flow injection analysis is presented. It has well developed the normal spectrofluorimetric method for determination of cerium and has made: 1, the determination procedure shortened; 2, the determination speed increased to about 180 samples per hour; 3, the determination range widened to 0.05-100.0 ppm CeO 2 , abouot two times as wide as the normal spectrofluorimetric method; and 4, the relative standard deviation lessened (about 0.47% for 0.1 ppm CeO 2 , n = 13)

  3. Flow Injection and Atomic Absorption Spectrometry (FI-AAS) -

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...... the point of sample injection/introduction to the point of detection. Hence, in FI-fAAS this feature allows not only to obtain improved repeatability but also improved accuracy, and because the wash to sample ratio is high it permits the handling of samples with elevated salt contents - which...

  4. Amperometric screen-printed algal biosensor with flow injection analysis system for detection of environmental toxic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Shitanda, Isao [Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba 278-8510 (Japan)], E-mail: shitanda@rs.noda.tus.ac.jp; Takamatsu, Satoshi; Watanabe, Kunihiro; Itagaki, Masayuki [Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba 278-8510 (Japan)

    2009-08-30

    A screen-printed algal biosensor was fabricated for evaluation of toxicity of chemicals. An algal ink was prepared by mixing unicellular microalga Chlorella vulgaris cells, carbon nanotubes and sodium alginate solution. The algal ink was immobilized directly on a screen-printed carbon electrode surface using screen-printing technique. Photosynthetically generated oxygen of the immobilized algae was monitored amperometically. Responses of the algal biosensor to four toxic compounds, 6-chloro-N-ethyl-N-isopropyl-1,3,5-triazine-2,4-diamine (atrazine) and 3-(3,4-dichlorophenyl)-1,1-diethylurea (DCMU) were evaluated as inhibition ratios of the reduction current. The concentrations that gave 50% inhibition of the oxygen reduction current (IC{sup '}{sub 50}) for atrazine and DCMU were 12 and 1 {mu}mol dm{sup -3}, respectively. In comparison with the conventional algal biosensors, in which the algal cells were entrapped in an alginate gel and immobilized on the surface of a transparent indium tin oxide electrode, the present sensor is much smaller and less expensive, with the shorter assay time.

  5. Amperometric screen-printed algal biosensor with flow injection analysis system for detection of environmental toxic compounds

    International Nuclear Information System (INIS)

    Shitanda, Isao; Takamatsu, Satoshi; Watanabe, Kunihiro; Itagaki, Masayuki

    2009-01-01

    A screen-printed algal biosensor was fabricated for evaluation of toxicity of chemicals. An algal ink was prepared by mixing unicellular microalga Chlorella vulgaris cells, carbon nanotubes and sodium alginate solution. The algal ink was immobilized directly on a screen-printed carbon electrode surface using screen-printing technique. Photosynthetically generated oxygen of the immobilized algae was monitored amperometically. Responses of the algal biosensor to four toxic compounds, 6-chloro-N-ethyl-N-isopropyl-1,3,5-triazine-2,4-diamine (atrazine) and 3-(3,4-dichlorophenyl)-1,1-diethylurea (DCMU) were evaluated as inhibition ratios of the reduction current. The concentrations that gave 50% inhibition of the oxygen reduction current (IC ' 50 ) for atrazine and DCMU were 12 and 1 μmol dm -3 , respectively. In comparison with the conventional algal biosensors, in which the algal cells were entrapped in an alginate gel and immobilized on the surface of a transparent indium tin oxide electrode, the present sensor is much smaller and less expensive, with the shorter assay time.

  6. FLOW INJECTION AMPEROMETRIC DETECTION OF OP NERVE AGENTS BASED ON AN ORGANOPHOSPHORUS-HYDROLASE BIOSENSOR DETECTOR. (R828160)

    Science.gov (United States)

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  7. Sensitive flow-injection spectrophotometric analysis of bromopride

    Science.gov (United States)

    Lima, Liliane Spazzapam; Weinert, Patrícia Los; Pezza, Leonardo; Pezza, Helena Redigolo

    2014-12-01

    A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax = 565 nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63 × 10-7 to 2.90 × 10-5 mol L-1, with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07 × 10-7 and 3.57 × 10-7 mol L-1, respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps.

  8. Flow injection spectrofluorimetric method for the determination of cadmium

    International Nuclear Information System (INIS)

    Bo Tang; Taixing Yue; Lili Zhang; Junsen Wu; Zhenzhen Chen

    2004-01-01

    A novel fluorescent reagent, o-vanillin furoylhydrazone (OVFH), was synthesized, and its infrared spectrum, elemental analysis and dissociation constant are reported. The reaction between Cd 2+ and OVFH produces an intensely fluorescent complex in ethanol-water medium of pH 10.00, and this finding has led to a simple, rapid, and sensitive flow injection (FI) spectrofluorimetric method for on-line determination of Cd 2+ . Under the optimum experimental conditions, the fluorescent complex had excitation and emission maxima at 393 and 494 nm, respectively. The linear range is from 0.025 to 8.0 μg mL -1 of Cd 2+ , the detection limit is 7.6 μg L -1 and the maximum sampling rate is 80 h -1 . The effect of interferences was studied. The method was successfully applied to the determination of cadmium in environmental samples. (author)

  9. Principles and Applications of Flow Injection Analysis in Biosensors

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1996-01-01

    In practical applications biosensors are often forced to operate under less than optimal conditions. Because of their construction, and the physical processes and chemical reactions involved in their operation, compromise conditions are frequently required to synchronize all events taking place....... Therefore, and in order to implement functions such as periodic calibration, conditioning and possible regeneration of the biosensor, and, very importantly, to yield the freedom to select the optimum detection means, it is advantageous to use these devices in a flow-through mode, particularly by employing...... the flow injection (FI) approach. The capacity of FI, as offering itself as a complementary facility to augment the performance of biosensors, and in many cases as an attractive alternative, is demonstrated by reference to selected examples, comprising assays based on enzymatic procedures with optical...

  10. Biosensing of glucose in flow injection analysis system based on glucose oxidase-quantum dot modified pencil graphite electrode.

    Science.gov (United States)

    Sağlam, Özlem; Kızılkaya, Bayram; Uysal, Hüseyin; Dilgin, Yusuf

    2016-01-15

    A novel amperometric glucose biosensor was proposed in flow injection analysis (FIA) system using glucose oxidase (GOD) and Quantum dot (ZnS-CdS) modified Pencil Graphite Electrode (PGE). After ZnS-CdS film was electrochemically deposited onto PGE surface, GOD was immobilized on the surface of ZnS-CdS/PGE through crosslinking with chitosan (CT). A pair of well-defined reversible redox peak of GOD was observed at GOD/CT/ZnS-CdS/PGE based on enzyme electrode by direct electron transfer between the protein and electrode. Further, obtained GOD/CT/ZnS-CdS/PGE offers a disposable, low cost, selective and sensitive electrochemical biosensing of glucose in FIA system based on the decrease of the electrocatalytic response of the reduced form of GOD to dissolved oxygen. Under optimum conditions (flow rate, 1.3mL min(-1); transmission tubing length, 10cm; injection volume, 100μL; and constant applied potential, -500mV vs. Ag/AgCl), the proposed method displayed a linear response to glucose in the range of 0.01-1.0mM with detection limit of 3.0µM. The results obtained from this study would provide the basis for further development of the biosensing using PGE based FIA systems. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Development of flow injection analysis technique for uranium estimation

    International Nuclear Information System (INIS)

    Paranjape, A.H.; Pandit, S.S.; Shinde, S.S.; Ramanujam, A.; Dhumwad, R.K.

    1991-01-01

    Flow injection analysis is increasingly used as a process control analytical technique in many industries. It involves injection of the sample at a constant rate into a steady flowing stream of reagent and passing this mixture through a suitable detector. This paper describes the development of such a system for the analysis of uranium (VI) and (IV) and its gross gamma activity. It is amenable for on-line or automated off-line monitoring of uranium and its activity in process streams. The sample injection port is suitable for automated injection of radioactive samples. The performance of the system has been tested for the colorimetric response of U(VI) samples at 410 nm in the range of 35 to 360mg/ml in nitric acid medium using Metrohm 662 Photometer and a recorder as detector assembly. The precision of the method is found to be better than +/- 0.5%. This technique with certain modifications is used for the analysis of U(VI) in the range 0.1-3mg/ailq. by alcoholic thiocynate procedure within +/- 1.5% precision. Similarly the precision for the determination of U(IV) in the range 15-120 mg at 650 nm is found to be better than 5%. With NaI well-type detector in the flow line, the gross gamma counting of the solution under flow is found to be within a precision of +/- 5%. (author). 4 refs., 2 figs., 1 tab

  12. Flow injection kinetic spectrofluorimetric determination of trace amounts of osmium

    Science.gov (United States)

    Tang, Bo; Zhang, Hui; Wang, Yan

    2005-07-01

    A flow injection (FI) kinetic spectrofluorimetric method is described for the determination of osmium(IV) and the possible mechanism of catalytic reaction is discussed. The method is based on the fluorescence enhancing reaction of o-vanillin furfuralhydrazone (OVFH) with potassium bromate, which is catalyzed by Os(IV) in water medium at pH 6.10 and 45 °C. OVFH is newly synthesized and its ionization, IR and elemental analysis are established. Under these experimental conditions, the oxidized product of OVFH has excitation and emission maxima at 337 and 490 nm, respectively. The linear range of this method is 0-600 ng ml -1 with the R.S.D. of 1.2%. The detection limit is 1.0 ng ml -1 of Os(IV). A high analysis rate of 24 samples h -1 is obtained by the FI method. The proposed method is applied successfully to determine Os(IV) in synthetic mixture and mineral samples, and the results are well consistent with the standard values.

  13. Remote calorimetric detection of urea via flow injection analysis.

    Science.gov (United States)

    Gaddes, David E; Demirel, Melik C; Reeves, W Brian; Tadigadapa, Srinivas

    2015-12-07

    The design and development of a calorimetric biosensing system enabling relatively high throughput sample analysis are reported. The calorimetric biosensor system consists of a thin (∼20 μm) micromachined Y-cut quartz crystal resonator (QCR) as a temperature sensor placed in close proximity to a fluidic chamber packed with an immobilized enzyme. Layer by layer enzyme immobilization of urease is demonstrated and its activity as a function of the number of layers, pH, and time has been evaluated. This configuration enables a sensing system where a transducer element is physically separated from the analyte solution of interest and is thereby free from fouling effects typically associated with biochemical reactions occuring on the sensor surface. The performance of this biosensing system is demonstrated by detection of 1-200 mM urea in phosphate buffer via a flow injection analysis (FIA) technique. Miniaturized fluidic systems were used to provide continuous flow through a reaction column. Under this configuration the biosensor has an ultimate resolution of less than 1 mM urea and showed a linear response between 0-50 mM. This work demonstrates a sensing modality in which the sensor itself is not fouled or contaminated by the solution of interest and the enzyme immobilized Kapton® fluidic reaction column can be used as a disposable cartridge. Such a system enables reuse and reliability for long term sampling measurements. Based on this concept a biosensing system is envisioned which can perform rapid measurements to detect biomarkers such as glucose, creatinine, cholesterol, urea and lactate in urine and blood continuously over extended periods of time.

  14. Flow injection analysis: Emerging tool for laboratory automation in radiochemistry

    International Nuclear Information System (INIS)

    Egorov, O.; Ruzicka, J.; Grate, J.W.; Janata, J.

    1996-01-01

    Automation of routine and serial assays is a common practice of modern analytical laboratory, while it is virtually nonexistent in the field of radiochemistry. Flow injection analysis (FIA) is a general solution handling methodology that has been extensively used for automation of routine assays in many areas of analytical chemistry. Reproducible automated solution handling and on-line separation capabilities are among several distinctive features that make FI a very promising, yet under utilized tool for automation in analytical radiochemistry. The potential of the technique is demonstrated through the development of an automated 90 Sr analyzer and its application in the analysis of tank waste samples from the Hanford site. Sequential injection (SI), the latest generation of FIA, is used to rapidly separate 90 Sr from interfering radionuclides and deliver separated Sr zone to a flow-through liquid scintillation detector. The separation is performed on a mini column containing Sr-specific sorbent extraction material, which selectively retains Sr under acidic conditions. The 90 Sr is eluted with water, mixed with scintillation cocktail, and sent through the flow cell of a flow through counter, where 90 Sr radioactivity is detected as a transient signal. Both peak area and peak height can be used for quantification of sample radioactivity. Alternatively, stopped flow detection can be performed to improve detection precision for low activity samples. The authors current research activities are focused on expansion of radiochemical applications of FIA methodology, with an ultimate goal of creating a set of automated methods that will cover the basic needs of radiochemical analysis at the Hanford site. The results of preliminary experiments indicate that FIA is a highly suitable technique for the automation of chemically more challenging separations, such as separation of actinide elements

  15. Wireless Amperometric Neurochemical Monitoring Using an Integrated Telemetry Circuit

    Science.gov (United States)

    Roham, Masoud; Halpern, Jeffrey M.; Martin, Heidi B.; Chiel, Hillel J.

    2015-01-01

    An integrated circuit for wireless real-time monitoring of neurochemical activity in the nervous system is described. The chip is capable of conducting high-resolution amperometric measurements in four settings of the input current. The chip architecture includes a first-order ΔΣ modulator (ΔΣM) and a frequency-shift-keyed (FSK) voltage-controlled oscillator (VCO) operating near 433 MHz. It is fabricated using the AMI 0.5 μm double-poly triple-metal n-well CMOS process, and requires only one off-chip component for operation. Measured dc current resolutions of ~250 fA, ~1.5 pA, ~4.5 pA, and ~17 pA were achieved for input currents in the range of ±5, ±37, ±150, and ±600 nA, respectively. The chip has been interfaced with a diamond-coated, quartz-insulated, microneedle, tungsten electrode, and successfully recorded dopamine concentration levels as low as 0.5 μM wirelessly over a transmission distance of ~0.5 m in flow injection analysis experiments. PMID:18990633

  16. Wireless amperometric neurochemical monitoring using an integrated telemetry circuit.

    Science.gov (United States)

    Roham, Masoud; Halpern, Jeffrey M; Martin, Heidi B; Chiel, Hillel J; Mohseni, Pedram

    2008-11-01

    An integrated circuit for wireless real-time monitoring of neurochemical activity in the nervous system is described. The chip is capable of conducting high-resolution amperometric measurements in four settings of the input current. The chip architecture includes a first-order Delta Sigma modulator (Delta Sigma M) and a frequency-shift-keyed (FSK) voltage-controlled oscillator (VCO) operating near 433 MHz. It is fabricated using the AMI 0.5 microm double-poly triple-metal n-well CMOS process, and requires only one off-chip component for operation. Measured dc current resolutions of approximately 250 fA, approximately 1.5 pA, approximately 4.5 pA, and approximately 17 pA were achieved for input currents in the range of +/-5, +/-37, +/-150, and +/-600 nA, respectively. The chip has been interfaced with a diamond-coated, quartz-insulated, microneedle, tungsten electrode, and successfully recorded dopamine concentration levels as low as 0.5 microM wirelessly over a transmission distance of approximately 0.5 m in flow injection analysis experiments.

  17. Flow injection analysis of sulphide based on its photoelectrocatalytic oxidation at poly-methylene blue modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Dilgin, Yusuf; Canarslan, Seda; Ayyildiz, Onder; Ertek, Bensu; Nişli, Gürel

    2012-01-01

    A new approach for photoelectrocatalytic determination of sulphide in a flow injection analysis (FIA) system was studied using a poly-methylene blue modified glassy carbon electrode (poly-MB/GCE). Results from electrochemical measurements have revealed that poly-MB/GCE is capable of signalling electrocatalytic and photoelectrocatalytic activity towards sulphide oxidation. When the surface of poly-MB/GCE was irradiated with a light source (250 W Halogen lamp), the electrocatalytic current increased substantially. A homemade flow electrochemical cell with a suitable transparent window for the irradiation of the electrode surface was used to perform the photoelectrocatalytic determination of sulphide in FIA system. The currents obtained from the photoamperometric measurements in the FIA system at optimum conditions (carrier solution: pH 9.0 Britton Robinson buffer solution containing 0.1 M KCl; flow rate: 1.3 mL min −1 ; transmission tubing length: 10 cm; injection volume: 100 μL; and constant applied potential: +150 mV vs. Ag/AgCl/KCl sat ) were linearly correlated with the sulphide concentration. The calibration curves were obtained for sulphide concentrations in a range of 0.5–500 μM. The detection limits were found to be 0.27 and 0.15 μM for amperometric and photoamperometric methods, respectively. The proposed method was successfully applied to different wastewaters such as municipal sewage or tannery wastewater. Finally, results from the sulphide measurements by poly-MB/GCE were in good agreement with those attained using spectrophotometric method.

  18. Carbon nanotube enhanced membrane distillation for online preconcentration of trace pharmaceuticals in polar solvents.

    Science.gov (United States)

    Gethard, Ken; Mitra, Somenath

    2011-06-21

    Carbon nanotube enhanced membrane distillation (MD) is presented as a novel, online analytical preconcentration method for removing polar solvents thereby concentrating the analytes, making this technique an alternate to conventional thermal evaporation. In a carbon nanotube immobilized membrane (CNIM), the CNTs serve as sorbent sites and provide additional pathways for enhanced solvent vapor transport, thus enhancing preconcentration. Enrichment using CNIM doubled compared to membranes without CNTs, while the methanol flux and mass transfer coefficients increased by 61% and 519% respectively. The carbon nanotube enhanced MD process showed excellent precision (RSD of 3-5%), linearity, and the detection limits were in the range of 0.001 to 0.009 mg L(-1) by HPLC analysis.

  19. Polymer based amperometric hydrogen sensor

    International Nuclear Information System (INIS)

    Ramesh, C.; Periaswami, G.; Mathews, C.K.; Shankar, P.

    1993-01-01

    A polymer based amperometric hydrogen sensor has been developed for measuring hydrogen in argon. Polyvinyl alcohol-phosphoric acid serves as the solid electrolyte for proton conduction. The electrolyte is sandwiched between two palladium films. Short circuit current between the film at room temperature is measured and is found to be linearly dependant on hydrogen concentration in argon to which one side of the film is exposed. The other side is exposed to air. The response time of the sensor is found to be improved on application of a D.C. potential of 200 mV in series. The sensitivity of the sensor is in ppm range. This may be sufficient for monitoring cover gas hydrogen in FBTR. Work is underway to improve the long-term stability of the sensor. (author)

  20. Carbon film resistor electrode for amperometric determination of acetaminophen in pharmaceutical formulations.

    Science.gov (United States)

    Felix, Fabiana S; Brett, Christopher M A; Angnes, Lúcio

    2007-04-11

    Flow injection analysis (FIA) with amperometric detection was employed for acetaminophen quantification in pharmaceutical formulations using a carbon film resistor electrode. This sensor exhibited sharp and reproducible current peaks for acetaminophen without chemical modification of its surface. A wide linear working range (8.0x10(-7) to 5.0x10(-4) mol L(-1)) in phosphate buffer solution as well as high sensitivity (0.143 A mol(-1) L cm(-2)) and low submicromolar detection limit (1.36x10(-7) mol L(-1)) were achieved. The repeatability (R.S.D. for 10 successive injections of 5.0x10(-6) and 5.0x10(-5) mol L(-1) acetaminophen solutions) was 3.1 and 1.3%, respectively, without any memory effect between injections. The new procedure was applied to the analyses of commercial pharmaceutical products and the results were in good agreement with those obtained utilizing a spectrophotometric method. Consequently, this amperometric method has been shown to be very suitable for quality control analyses and other applications with similar requirements.

  1. Automated amperometric plutonium assay system

    International Nuclear Information System (INIS)

    Burt, M.C.

    1985-01-01

    The amperometric titration for plutonium assay has been used in the nuclear industry for over twenty years and has been in routine use at the Hanford Engineering Development Laboratory since 1976 for the analysis of plutonium oxide and mixed oxide fuel material for the Fast Flux Test Facility. It has proven itself to be an accurate and reliable method. The method may be used as a direct end point titration or an excess of titrant may be added and a back titration performed to aid in determination of the end point. Due to the slowness of the PuVI-FeII reaction it is difficult to recognize when the end point is being approached and is very time consuming if the current is allowed to decay to the residual value after each titrant addition. For this reason the back titration in which the rapid FeII-CrVI reaction occurs is used by most laboratories. The back titration is performed by the addition of excess ferrous solution followed by two measured aliquots of standard dichromate with measurement of cell current after each addition

  2. Micro-flow-injection analysis (μFIA) immunoassay of herbicide residue 2,6-dichlorobenzamide

    DEFF Research Database (Denmark)

    Uthuppu, Basil; Heiskanen, Arto; Kofoed, Dan

    2015-01-01

    As a part of developing new systems for continuously monitoring the presence of pesticides in groundwater, a microfluidic amperometric immunosensor was developed for detecting the herbicide residue 2,6-dichlorobenzamide (BAM) in water. A competitive immunosorbent assay served as the sensing mecha...

  3. Flow Injection and Atomic Absorption Spectrometry - An Effective and Attractive Analytical Chemical Combination

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Nielsen, Steffen

    1998-01-01

    One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atom...

  4. Wavelet transform for the evaluation of peak intensities in flow-injection analysis

    NARCIS (Netherlands)

    Bos, M.; Hoogendam, E.

    1992-01-01

    The application of the wavelet transform in the determination of peak intensities in flow-injection analysis was studied with regard to its properties of minimizing the effects of noise and baseline drift. The results indicate that for white noise and a favourable peak shape a signal-to-noise ratio

  5. Wavelett transform for the evaluation of peak intensities in flow-injection analysis

    NARCIS (Netherlands)

    Bos, M.; Hoogendam, E.; Hoogendam, E.

    1992-01-01

    The application of the wavelet transform in the determination of peak intensities in flow-injection analysis was studied with regard to its properties of minimizing the effects of noise and baseline drift. The results indicate that for white noise and a favourable peak shape a signal-to-noise ratio

  6. Reverse radiometric flow injection analysis (RFIA) of radioactive waste-waters with an ASIA (Ismatec) analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Myint, U; Win, N; San, K; Han, B; Myoe, K M [Yangon Univ. (Myanmar). Dept. of Chemistry; Toelgyessy, J [Slovak Technical Univ., Bratislava (Slovakia). Dept. of Environmental Science

    1994-07-01

    A new application of reverse radiometric flow injection analysis is described. RFIA was used for the analysis of radioactive wastewaters. ASIA (Ismatec) analyzer with NaI(Tl) scintillation detector was used in the study of analysis of [sup 131]I containing waste-aster. (author) 4 refs.; 3 figs.

  7. Sequential injection lab-on-valve: the third generation of flow injection analysis

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    Termed the third generation of flow injection analysis, sequential injection (SI)-lab-on-valve (LOV) has specific advantages and allows novel, unique applications - not least as a versatile front end to a variety of detection techniques. This review presents snd discusses progress to date of the ...

  8. Determination of uranium (IV) in cloride solutions of enrichment columns by spectrometry with flow injection

    International Nuclear Information System (INIS)

    Bastos, M.B.R.

    1988-01-01

    The utilization of Flow Injection Analysis for the U (IV) spectrophotometric determination in chloride solutions is described. The method has been shown reproducible in the range of concentrations and conditions employed with a standard deviation of about 0,3. (C.G.C.) [pt

  9. Amperometric Noise at Thin Film Band Electrodes

    DEFF Research Database (Denmark)

    Larsen, Simon T.; Heien, Michael L.; Taboryski, Rafael

    2012-01-01

    Background current noise is often a significant limitation when using constant-potential amperometry for biosensor application such as amperometric recordings of transmitter release from single cells through exocytosis. In this paper, we fabricated thin-film electrodes of gold and conductive...

  10. Recent Development in Optical Chemical Sensors Coupling with Flow Injection Analysis

    Directory of Open Access Journals (Sweden)

    Fuensanta Sánchez Rojas

    2006-10-01

    Full Text Available Optical techniques for chemical analysis are well established and sensors based on thesetechniques are now attracting considerable attention because of their importance in applications suchas environmental monitoring, biomedical sensing, and industrial process control. On the other hand,flow injection analysis (FIA is advisable for the rapid analysis of microliter volume samples and canbe interfaced directly to the chemical process. The FIA has become a widespread automatic analyticalmethod for more reasons; mainly due to the simplicity and low cost of the setups, their versatility, andease of assembling. In this paper, an overview of flow injection determinations by using opticalchemical sensors is provided, and instrumentation, sensor design, and applications are discussed. Thiswork summarizes the most relevant manuscripts from 1980 to date referred to analysis using opticalchemical sensors in FIA.

  11. Theoretical considerations of Flow Injection Analysis in the Absence of Chemical Reactions

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    2000-01-01

    The fundamental mechanism of flow injection analysis (FIA) is assumed to be simple dissusion and the response of the detector is included in a model description that provide information about the shape of the FIA peak in terms of, basically, five parameters. Two of the five parameters are associa...... that any deviation from the features of the present model and the results of a tentative chemical reaction with one of the test compounds, is related to chemical kinetics.......The fundamental mechanism of flow injection analysis (FIA) is assumed to be simple dissusion and the response of the detector is included in a model description that provide information about the shape of the FIA peak in terms of, basically, five parameters. Two of the five parameters...

  12. Spectrophotometric flow injection catalytic determination of molybdenum in plant digest using ion exchange resin

    International Nuclear Information System (INIS)

    Pessenda, L.C.R.

    1987-03-01

    A spectrophotometric flow injection analytical method based on the catalytic action of molybdenum on the oxidation of iodide by hydrogen peroxide in acidic medium is proposed for the molybdenum determination in plant digests. A cation exchange resin column is incorporated into a flow injection system for removal of interferents. The following system variables were investigated and optimized: reagent concentrations, sample injection volume, mixing and reaction coil lengths, temperature, sampling time, pumping rate and concentration of eluting agents. The effects of interfering species and of the acidity of samples on the molybdenum retention by the ion exchange resin column were investigated. The proposed method is characterized by good precision (r.s.d. (2.0%), a sampling rate of about 40 samples per hour, and permits the determination of molybdenum in plant digests in the range 1.0 to 40.0 μg/l. The results compare well with those obtained by graphite furnace atomic absorption spectrometry. (author) [pt

  13. Mathematical modeling of flow-injection techniques and their applications for environmental monitoring

    International Nuclear Information System (INIS)

    Begum, N.N.; Ahmed, J.

    2006-01-01

    A classification of the existing mathematical models of flow-injection (FI) manifolds based on the main principles on which they are built, have been proposed. Numerous mathematical models of FI systems employing ideas from different scientific areas (e.g. mathematical statistics, chemical engineering, chromatography) have been developed so far. The models have been compared with respect to their predictive power, the complexity of their mathematical treatment, and the requirements for computation time when applied to single-line, multi-channel and conjugated two-line FI systems. It is concluded that the axially dispersed plug flow model deserves special attention because it offers an acceptable compromise between the conflicting requirements for maximal possible mathematical simplicity and maximal possible precision. Applicability of these existing flow-injection models to single-line, multi-channel and conjugated two-line systems for environmental monitoring have been discussed. (author)

  14. Enzymatic amplification of a flow-injected thermometric enzyme-linked immunoassay for human insulin.

    Science.gov (United States)

    Mecklenburg, M; Lindbladh, C; Li, H; Mosbach, K; Danielsson, B

    1993-08-01

    A flow-injected thermometric enzyme linked immunoassay for human insulin which employs the lactate dehydrogenase/lactate oxidase (LDH/LOD) substrate recycling system for signal amplification is described. The system is composed of two columns, an immunosorbent column containing immobilized anti-insulin antibodies for sensing and a recycling column containing immobilized LDH/LOD/Catalase for detection. The effect of flow rates, conjugate concentrations, and chromatographic support material upon the sensitivity of the assay are investigated. The assay has a detection limit of 0.025 microgram/ml and a linear range from 0.05 to 2 micrograms/ml. This corresponds to a 10-fold increase in sensitivity over the unamplified system. A recombinant human insulin-proinsulin conjugate was also tested. The results show that enzymatic amplification can be employed to increase the sensitivity and reproducibility of flow injection assay-based biosensors. The implications of these results upon on-line analysis are discussed.

  15. Stopped-flow injection spectrophotometric method for determination of chlorate in soil

    OpenAIRE

    Jaroon Jakmunee

    2008-01-01

    A stopped-flow injection (FI) spectrophotometric procedure based on iodometric reaction for the determination of chlorate has been developed. Standard/sample was injected into a stream of potassium iodide solution and then merged with a stream of hydrochloric acid solution to produce triiodide. By stopping the flow while the sample zone is being in a mixing coil, a slow reaction of chlorate with iodide in acidic medium was promoted to proceed with minimal dispersion of the triiodide product z...

  16. The determination, by flow-injection analysis, of iron, sulphate, silver and cadmium

    International Nuclear Information System (INIS)

    Jones, E.A.

    1983-01-01

    This report describes the spectrophotometric determination by flow-injection analysis including, where necessary, liquid-liquid extraction of iron with 1,10-phenanthroline; of sulphate by its catalytic effect on the methylthymol blue-zirconium reaction; of silver with bromopyrogallol red and 1,10-phenanthroline; and of cadmium with dithizone. Optimum conditions for each system are established, and sensitivities and ranges of determination are given

  17. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

  18. Micelle-mediated methodology for the preconcentration of uranium prior to its determination by flow injection

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez Laespada, M E; Perez Pavon, J L; Moreno Cordero, B [Univ. de Salamanca (Spain). Dept. de Quimica Analitica, Nutricion y Bromatologia

    1993-02-01

    Cloud point extraction has been used for the preconcentration of uranium, prior to its determination by flow injection. The non-ionic surfactant employed was Triton X-114 and the reagent chosen to form a hydrophobic chelate of uranium was 1-(2-pyridylazo)-2-naphthol. The optimum conditions for the preconcentration and determination of uranium have been studied. This methodology has been applied to the determination of trace amounts of uranium in tap and river waters from Salamanca. (Author).

  19. Determination of albumin in bronchoalveolar lavage fluid by flow-injection fluorometry using chromazurol S.

    Science.gov (United States)

    Sato, Takaji; Saito, Yoshihiro; Chikuma, Masahiko; Saito, Yutaka; Nagai, Sonoko

    2008-03-01

    A highly sensitive flow injection fluorometry for the determination of albumin was developed and applied to the determination of albumin in human bronchoalveolar lavage fluids (BALF). This method is based on binding of chromazurol S (CAS) to albumin. The calibration curve was linear in the range of 5-200 microg/ml of albumin. A highly linear correlation (r=0.986) was observed between the albumin level in BALF samples (n=25) determined by the proposed method and by a conventional fluorometric method using CAS (CAS manual method). The IgG interference was lower in the CAS flow injection method than in the CAS manual method. The albumin level in BALF collected from healthy volunteers (n=10) was 58.5+/-13.1 microg/ml. The albumin levels in BALF samples obtained from patients with sarcoidosis and idiopathic pulmonary fibrosis were increased. This finding shows that the determination of albumin levels in BALF samples is useful for investigating lung diseases and that CAS flow injection method is promising in the determination of trace albumin in BALF samples, because it is sensitive and precise.

  20. Application of Ionic Liquids in Amperometric Gas Sensors.

    Science.gov (United States)

    Gębicki, Jacek; Kloskowski, Adam; Chrzanowski, Wojciech; Stepnowski, Piotr; Namiesnik, Jacek

    2016-01-01

    This article presents an analysis of available literature data on metrological parameters of the amperometric gas sensors containing ionic liquids as an electrolyte. Four mechanism types of signal generation in amperometric sensors with ionic liquid are described. Moreover, this article describes the influence of selected physico-chemical properties of the ionic liquids on the metrological parameters of these sensors. Some metrological parameters are also compared for amperometric sensors with GDE and SPE electrodes and with ionic liquids for selected analytes.

  1. Electrochemical evaluation of the a carbon-paste electrode modified with spinel manganese(IV) oxide under flow conditions for amperometric determination of lithium

    International Nuclear Information System (INIS)

    Raymundo-Pereira, Paulo A.; Martin, Cibely S.; Bergamini, Marcio F.; Bocchi, Nerilso; Teixeira, Marcos F.S.

    2011-01-01

    The participation of cations in redox reactions of manganese oxides provides an opportunity for development of chemical sensors for non-electroactive ions. This paper describes the amperometric determination of lithium ions using carbon-paste electrode modified with spinel manganese(IV) oxide under flow conditions. Systematic investigations were made to optimize the experimental parameters for lithium sensor by flow injection analysis. The detection was based on the measurement of anodic current generated by oxidation of Mn(III) to Mn(IV) at the surface of the electrode and consequently the lithium ions extraction into the spinel structure. An operating potential of 0.50 V (vs. Ag/AgCl/3 KCl mol/L) was exploited for amperometric monitoring. The amperometric signal was linearly dependent on the lithium ions concentration over the range 4.0 x 10 -5 to 1.0 x 10 -3 mol L -1 . The equilibrium constant of insertion/extraction of the lithium ion in the spinel structure, apparent Gibbs energy of insertion, and surface coverage of the electrode with manganese oxide, were calculated by peak charge (Q) in different concentration under flow conditions. Considering selectivity, the peak charge of the sensor was found to be linearly dependent on the ionic radius of the alkaline and earth-alkaline cations.

  2. Determination of uranium by an amperometric method

    International Nuclear Information System (INIS)

    John, Mary; Venkataramana, P.; Vaidyanathan, S.; Natarajan, P.R.

    1981-01-01

    An amperometric method has been standardised for the determination of uranium. Uranium is reduced to its quadrivalent state in concentrated phosphoric acid medium with ferrous iron. The excess iron is destroyed with nitric acid in presence of Mo(VI). The medium is diluted and U(IV) is titrated with standard potassium dichromate to an amperometric end point using a pair of identical plantinum wires as electrodes. The reagent volumes and uranium quantities have been scaled down to 30 ml. and 2-5 mg of uranium in the present work with a view to minimising the problems associated with recovery of plutonium. The results are quantitative with an R.S.D. of 0.2% in the present version of weight based titrations. (author)

  3. Flow-injection system for automated dissolution testing of isoniazid tablets with chemiluminescence detection.

    Science.gov (United States)

    Li, B; Zhang, Z; Liu, W

    2001-05-30

    A simple and sensitive flow-injection chemiluminescence (CL) system for automated dissolution testing is described and evaluated for monitoring of dissolution profiles of isoniazid tablets. The undissolved suspended particles in the dissolved solution were eliminated via on-line filter. The novel CL system of KIO(4)-isoniazid was also investigated. The sampling frequency of the system was 120 h(-1). The dissolution profiles of isoniazid fast-release tablets from three sources were determined, which demonstrates the stability, great sensitivity, large dynamic measuring range and robustness of the system.

  4. Flow injection spectrophotometric determination of low concentrations of orthosphate in natural waters employing ion exchange resin

    International Nuclear Information System (INIS)

    Pessenda, L.C.R.

    1981-01-01

    A simple and fast method for the determination of low concentrations of orthophosphate in natural waters is described. Ion exchange is incorporated into a flow injection system by usina a resin column in the sample loop of a proportion injector. Effects of sample aspiration rate, sampling time, eluting agent concentration, pumping rate of the sample carrier stream and interfaces, were investigated both using 32 PO 3- 4 or 31 PO 3- 4 with columns coupled to a gerger-muller detector and incorporated in a flow system with molybdenum blue colorinetry. (M.A.C.) [pt

  5. [Determination of mercury in Boletus impolitus by flow injection-atomic absorption spectrometry].

    Science.gov (United States)

    Li, Tao; Wang, Yuan-Zhong

    2008-04-01

    Various test conditions and effect factors for the determination of mercury by flow injection-atomic absorption spectrometry were discussed, and a method for the determination of mercury in Boletus impolitus has been developed. The linear range for mercury is 0-60 microg x L(-1). The relative standard deviation is less than 3.0%, and the recovery is 96%-107%. This method is simple, rapid and has been applied to the determination of mercury in Boletus impolitus samples with satisfactory results.

  6. The determination of uranium(VI) by flow-injection analysis

    International Nuclear Information System (INIS)

    Jones, E.A.

    1985-01-01

    A method is described for the direct determination of uranium(VI) in waste waters and acid leach liquors by use of a flow-injection procedure and spectrophotometric measurement with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (bromo-PADAP). The interference effects of several commonly occurring elements were studied. The calibration curve is linear over concentrations of uranium(VI) from 0,5 to 20 mg/1, and the precision obtained on a synthetic leach liquor was 0,019 (relative standard deviation). The procedure is rapid and convenient, and up to 40 samples can be analysed in an hour

  7. Spectrophotometric determination of phosphorus in iron alloys employing a flow injection system

    OpenAIRE

    Gervasio,Ana P. G.; Miranda,Carlos E. S.; Luca,Gilmara C.; Tumang,Cristiane A.; Campos,Luis F. P.; Reis,Boaventura F.

    2001-01-01

    A flow-injection procedure for spectrophotometric determination of phosphorus in electrolytic iron and iron alloys is proposed. The method is based on the ammonium molybdate reaction followed by stannous chloride reduction in acidic medium. In order to circumvent the severe interference caused by the major constituents such as Fe(III) and Cr(III), a mini-column packed with AG50W-X8 resin was coupled to the manifold. A sample throughput of 40 determinations per hour, a dynamical range from P 0...

  8. Optimization of a flow injection analysis system for multiple solvent extraction

    International Nuclear Information System (INIS)

    Rossi, T.M.; Shelly, D.C.; Warner, I.M.

    1982-01-01

    The performance of a multistage flow injection analysis solvent extraction system has been optimized. The effect of solvent segmentation devices, extraction coils, and phase separators on performance characteristics is discussed. Theoretical consideration is given to the effects and determination of dispersion and the extraction dynamics within both glass and Teflon extraction coils. The optimized system has a sample recovery similar to an identical manual procedure and a 1.5% relative standard deviation between injections. Sample throughput time is under 5 min. These characteristics represent significant improvements over the performance of the same system before optimization. 6 figures, 2 tables

  9. Minicolumn field preconcentration and flow-injection flame atomic absorption spectrometric determination of cadmium in seawater

    International Nuclear Information System (INIS)

    Yebra-Biurrun, M.C.; Moreno-Cid, A.; Puig, L.

    2004-01-01

    A simple method for the continuous field preconcentration of trace dissolved cadmium in seawater samples has been developed based on the minicolumn field sampling technique. For this purpose, minicolumns containing Chelite P (aminomethylphosphonic groups) were connected to a field flow preconcentration system (FFPS). Once in the laboratory, these minicolumns are sequentially inserted into a flow-injection system for on-line cadmium elution and detection by flame atomic absorption spectrometry. Factorial designs have been used to optimise the FFPS and the flow-injection elution process. Six experimental variables were optimised: sample pH, sample flow-rate, eluent concentration, eluent volume, eluent flow-rate and minicolumn diameter. The detection limit (3F) of the procedure was 2.7 ng l -1 for a sample volume of 300 ml. The precision (expressed as relative standard deviation) for 11 independent determinations was 0.5-9.4% for cadmium solutions of 10-300 ng l -1 . Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified values. This procedure has been successfully applied to the determination of cadmium in seawater samples from Galicia (Spain)

  10. Indirect flow injection determination of N-acetyl-L-cysteine using cerium(IV) and ferroin

    International Nuclear Information System (INIS)

    Vieira, Heberth Juliano; Fatibello-Filho, Orlando

    2005-01-01

    An indirect flow injection spectrophotometric procedure is proposed for the determination of N-acetyl-L-cysteine in pharmaceutical formulations. In this system, ferroin ([Fe(II)-(fen) 2 ] 2+ ) in excess, with a strong absorption at 500 nm, is oxidized by cerium(IV) yielding cerium(III) and [Fe(III)-(fen) 2 ] 3+ (colorless), thus producing a baseline. When N-acetyl-L-cysteine solution is introduced into the flow injection system, it reacts with cerium(IV) increasing the analytical signal in proportion to the drug concentration. Under optimal experimental conditions, the linearity of the analytical curve for N-acetyl-L-cysteine ranged from 6.5x10 -6 to 1.3x10 -4 mol L -1 . The detection limit was 5.0x10 -6 mol L -1 and recoveries between 98.0 and 106% were obtained. The sampling frequency was 60 determinations per hour and the RSD was smaller than 1.4% for 2.2x10 -5 mol L -1 N-acetyl-L-cysteine. (author)

  11. Determination of pH by flow-injection analysis and by fiber-optrode analysis

    International Nuclear Information System (INIS)

    Pia, S.H.; Waltman, D.P.; Hillman, D.C.

    1988-07-01

    Two new procedures for measuring pH were developed. The first measures pH colorimetrically using a proprietary indicator-dye mixture in a flow injection analysis (FIA) procedure. The second measures pH using a fiber-optic chemical sensor (FOCS) specifically developed for pH determinations. The FOCS method measures pH by monitoring the fluorescence of a fluorescein derivative bonded to the distal end of a fiber-optic cable called an optrade. The FIA method currently has a precision and accuracy of about + or - 0.2 pH units and can measure 100 samples/hour. The FOCS method has a precision of + or - 0.05-0.20 pH units and an accuracy of + or - 0.1 to 0.6 pH units. About 10 to 60 samples can be analyzed. The characteristics of the FOCS Method will vary significantly with individual optrodes. The experimental results indicate that either flow-injection analysis or fiber optic chemical sensor analysis could form the basis for an alternative to electrometric measurement of pH in certain circumstances

  12. Dispersion-convolution model for simulating peaks in a flow injection system.

    Science.gov (United States)

    Pai, Su-Cheng; Lai, Yee-Hwong; Chiao, Ling-Yun; Yu, Tiing

    2007-01-12

    A dispersion-convolution model is proposed for simulating peak shapes in a single-line flow injection system. It is based on the assumption that an injected sample plug is expanded due to a "bulk" dispersion mechanism along the length coordinate, and that after traveling over a distance or a period of time, the sample zone will develop into a Gaussian-like distribution. This spatial pattern is further transformed to a temporal coordinate by a convolution process, and finally a temporal peak image is generated. The feasibility of the proposed model has been examined by experiments with various coil lengths, sample sizes and pumping rates. An empirical dispersion coefficient (D*) can be estimated by using the observed peak position, height and area (tp*, h* and At*) from a recorder. An empirical temporal shift (Phi*) can be further approximated by Phi*=D*/u2, which becomes an important parameter in the restoration of experimental peaks. Also, the dispersion coefficient can be expressed as a second-order polynomial function of the pumping rate Q, for which D*(Q)=delta0+delta1Q+delta2Q2. The optimal dispersion occurs at a pumping rate of Qopt=sqrt[delta0/delta2]. This explains the interesting "Nike-swoosh" relationship between the peak height and pumping rate. The excellent coherence of theoretical and experimental peak shapes confirms that the temporal distortion effect is the dominating reason to explain the peak asymmetry in flow injection analysis.

  13. O-(β-hydroxyethylrutosides determination by micellar flow injection (FI-spectrofluorimetry

    Directory of Open Access Journals (Sweden)

    Cecilia Mariana Peralta

    2014-12-01

    Full Text Available A simple, eco-friendly, sensitive and economic flow injection spectrofluorimetric method was developed for the determination of O-(β-hydroxyethylrutosides. The procedure was based on the use of an anionic surfactant such as sodium dodecyl sulfate to provide an appreciable O-(β-hydroxyethylrutosides fluorescence enhancement, increasing considerably the sensitivity of detection. All the variables affecting the fluorescence intensity were studied and optimized. The flow rate was 5 mL/min with detection at 450 nm (after excitation at 346 nm. A linear correlation between drug amount and peak area was established for O-(β-hydroxyethylrutosides in the range of 0.01–200 µg/mL with a detection limit of 0.001 µg/mL (s/n=3. Validation processes were performed by recovering studies with satisfactory results. The new methodology can be employed for the routine analysis of O-(β-hydroxyethylrutosides in bulks as well as in commercial formulations. Keywords: O-(β-hydroxyethylrutosides, Micellar enhancement, Flow injection, Spectrofluorimetry, Pharmaceuticals

  14. Fast cholesterol detection using flow injection microfluidic device with functionalized carbon nanotubes based electrochemical sensor.

    Science.gov (United States)

    Wisitsoraat, A; Sritongkham, P; Karuwan, C; Phokharatkul, D; Maturos, T; Tuantranont, A

    2010-12-15

    This work reports a new cholesterol detection scheme using functionalized carbon nanotube (CNT) electrode in a polydimethylsiloxane/glass based flow injection microfluidic chip. CNTs working, silver reference and platinum counter electrode layers were fabricated on the chip by sputtering and low temperature chemical vapor deposition methods. Cholesterol oxidase prepared in polyvinyl alcohol solution was immobilized on CNTs by in-channel flow technique. Cholesterol analysis based on flow injection chronoamperometric measurement was performed in 150-μm-wide and 150-μm-deep microchannels. Fast and sensitive real-time detection was achieved with high throughput of more than 60 samples per hour and small sample volume of 15 μl. The cholesterol sensor had a linear detection range between 50 and 400 mg/dl. In addition, low cross-sensitivities toward glucose, ascorbic acid, acetaminophen and uric acid were confirmed. The proposed system is promising for clinical diagnostics of cholesterol with high speed real-time detection capability, very low sample consumption, high sensitivity, low interference and good stability. Copyright © 2010 Elsevier B.V. All rights reserved.

  15. Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

    Science.gov (United States)

    Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

    2017-11-01

    An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Amperometric biosensor for the detection of hydrogen peroxide using catalase modified electrodes in polyacrylamide.

    Science.gov (United States)

    Varma, Shailly; Mattiasson, Bo

    2005-09-23

    A simple biosensor for the detection of hydrogen peroxide in organic solvents has been developed and coupled to a flow injection analysis (FIA) system. Catalase was entrapped in polyacrylamide gel and placed on the surface of platinum (working electrode) fixed in a Teflon holder with Ag-wire (auxiliary electrode), followed by addition of filter paper soaked in KCl. The entrapped catalase gel was held on the electrode using membranes. The effects of cellulose and polytetrafluroethylene (PTFE) membranes on the electrode response towards hydrogen peroxide have been studied. The modified electrode has been used to study the detection of hydrogen peroxide in solvents like water, dimethyl sulfoxide (DMSO), and 1,4-dioxane using amperometric techniques like cyclic voltammetry (CV) and FIA. The CV of modified catalase electrode showed a broad oxidation peak at -150 mV and a clear reduction peak at -212 mV in the presence of hydrogen peroxide. Comparison of CV with hydrogen peroxide in various solvents has been carried out. The electrode showed an irreversible kinetics with DMSO as the solvent. A flow cell has been designed in order to carry on FIA studies to obtain calibration plots for hydrogen peroxide with the modified electrode. The calibration plots in several solvents such as water, dimethyl sulfoxide, 1,4-dioxane have been obtained. The throughput of the enzyme electrode was 10 injections per hour. Due to the presence of membrane the response time of the electrode is concentration dependent.

  17. Bienzymatic Biosensor for Rapid Detection of Aspartame by Flow Injection Analysis

    Directory of Open Access Journals (Sweden)

    Maria-Cristina Radulescu

    2014-01-01

    Full Text Available A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX, carboxyl esterase (CaE and bovine serum albumin (BSA were immobilised with glutaraldehyde (GA onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC. The biosensor response was fast. The sample throughput using a flow injection analysis (FIA system was 40 h−1 with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 µM for methanol and 0.2 µM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples without any pre-treatment step prior to measurement.

  18. Method for 236U Determination in Seawater Using Flow Injection Extraction Chromatography and Accelerator Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Steier, Peter

    2015-01-01

    An automated analytical method implemented in a flow injection (FI) system was developed for rapid determination of 236U in 10 L seawater samples. 238U was used as a chemical yield tracer for the whole procedure, in which extraction chromatography (UTEVA) was exploited to purify uranium, after...... experimental parameters affecting the analytical effectiveness were investigated and optimized in order to achieve high chemical yields and simple and rapid analysis as well as low procedure background. Besides, the operational conditions for the target preparation prior to the AMS measurement were optimized......, on the basis of studying the coprecipitation behavior of uranium with iron hydroxide. The analytical results indicate that the developed method is simple and robust, providing satisfactory chemical yields (80−100%) and high analysis speed (4 h/sample), which could be an appealing alternative to conventional...

  19. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow.......g., soils, sediments, sludges), and thus, ascertaining the potential mobility, bioavailability and eventual impact of anthropogenic elements on biota [2]. In this context, the principles of sequential injection-microcolumn extraction (SI-MCE) for dynamic fractionation are explained in detail along...

  20. Home-Made Micro Valve for Determining Malachite Green Dye by Flow Injection Analysis

    Directory of Open Access Journals (Sweden)

    Amal Saadoon Majeed

    2017-07-01

    Full Text Available The research is included studying and designing micro flow injection system which is characterized with rapidity, simplicity, and low cost for the determination of green malachite dye. The study of flow rate of carrier stream, repeatability, dispersion coefficient, and calibration graph are conducted. It is found that the optimum conditions for the determination of mentioned dye are flow rate 4.200 mL/min, sampling rate 102 sample/h, limit of detection 0.05 ppm, linear range (0.05-18.00 ppm with linearity (R2=0.9700, RSD is 0.355, the repeatability for seven successive injections is studied for the two concentrations 5 ppm and 12 ppm, and the dispersion coefficient values are 1.73 and 1.28 at the two concentrations 2 ppm and 9 ppm respectively.

  1. Flow injection analysis simulations and diffusion coefficient determination by stochastic and deterministic optimization methods.

    Science.gov (United States)

    Kucza, Witold

    2013-07-25

    Stochastic and deterministic simulations of dispersion in cylindrical channels on the Poiseuille flow have been presented. The random walk (stochastic) and the uniform dispersion (deterministic) models have been used for computations of flow injection analysis responses. These methods coupled with the genetic algorithm and the Levenberg-Marquardt optimization methods, respectively, have been applied for determination of diffusion coefficients. The diffusion coefficients of fluorescein sodium, potassium hexacyanoferrate and potassium dichromate have been determined by means of the presented methods and FIA responses that are available in literature. The best-fit results agree with each other and with experimental data thus validating both presented approaches. Copyright © 2013 The Author. Published by Elsevier B.V. All rights reserved.

  2. Irreversibility analysis of magneto-hydrodynamic nanofluid flow injected through a rotary disk

    Directory of Open Access Journals (Sweden)

    Rashidi Mohammad Mehdi

    2015-01-01

    Full Text Available The non-linear Navier-Stokes equations governed on the nanofluid flow injected through a rotary porous disk in the presence of an external uniform vertical magnetic field can be changed to a system of non-linear partial differential equations by applying similar parameter. In this study, partial differential equations are analytically solved by the modified differential transform method, Pade differential transformation method to obtain self-similar functions of motion and temperature. A very good agreement is observed between the obtained results of Pade differential transformation method and those of previously published ones. Then it has become possible to do a comprehensive parametric analysis on the entropy generation in this case to demonstrate the effects of physical flow parameters such as magnetic interaction parameter, injection parameter, nanoparticle volume fraction, dimensionless temperature difference, rotational Brinkman number and the type of nanofluid on the problem.

  3. Optimized and validated flow-injection spectrophotometric analysis of topiramate, piracetam and levetiracetam in pharmaceutical formulations.

    Science.gov (United States)

    Hadad, Ghada M; Abdel-Salam, Randa A; Emara, Samy

    2011-12-01

    Application of a sensitive and rapid flow injection analysis (FIA) method for determination of topiramate, piracetam, and levetiracetam in pharmaceutical formulations has been investigated. The method is based on the reaction with ortho-phtalaldehyde and 2-mercaptoethanol in a basic buffer and measurement of absorbance at 295 nm under flow conditions. Variables affecting the determination such as sample injection volume, pH, ionic strength, reagent concentrations, flow rate of reagent and other FIA parameters were optimized to produce the most sensitive and reproducible results using a quarter-fraction factorial design, for five factors at two levels. Also, the method has been optimized and fully validated in terms of linearity and range, limit of detection and quantitation, precision, selectivity and accuracy. The method was successfully applied to the analysis of pharmaceutical preparations.

  4. Photometric estimation of plutonium in product solutions and acid waste solutions using flow injection analysis technique

    International Nuclear Information System (INIS)

    Dhas, A.J.A.; Dharmapurikar, G.R.; Kumaraguru, K.; Vijayan, K.; Kapoor, S.C.; Ramanujam, A.

    1995-01-01

    Flow injection analysis technique is employed for the measurement of plutonium concentrations in product nitrate solutions by measuring the absorbance of Pu(III) at 565 nm and of Pu(IV) at 470 nm, using a Metrohm 662 photometer, with a pyrex glass tube of 2 nm (ID) inserted in the light path of the detector serving as a flow cell. The photometer detector never comes in contact with radioactive solution. In the case of acid waste solutions Pu is first purified by extraction chromatography with 2-ethyl hexyl hydrogen 2 ethyl hexyl phosphonate (KSM 17)- chromosorb and the Pu in the eluate in complexed with Arsenazo III followed by the measured of absorbance at 665 nm. Absorbance of reference solutions in the desired concentration ranges are measured to calibrate the system. The results obtained agree with the reference values within ±2.0%. (author). 3 refs., 1 tab

  5. Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m...... of 10-30 were obtained in the analysis of aluminium, of chromium and of iron, which resulted in detection limits (3) down to 20 g/L at a sampling frequency of 50 per hour. The preconcentration protocol improves the selectivity thus allowing direct determination of the elements in saline media. Anionic...

  6. Sibutramine selective electrodes for batch and flow injection determinations in pharmaceutical preparations.

    Science.gov (United States)

    Zayed, S I M; Issa, Y M

    2010-01-01

    The construction and electrochemical response characteristics of two new polyvinyl chloride (PVC) membrane sensors for the determination of sibutramine hydrochloride were described. The sensors are based on the ion association complexes of sibutramine with sodium tetraphenylborate (NaTPB) or phosphotungstic acid (PTA) using dibutyl phthalate as plasticizing solvent. The sensors display a fast, stable response over the concentration range 3.84 x 10(-5)-1.00 x 10(-2) M sibutramine hydrochloride monohydrate (SibuCl), with cationic slopes of 57.7 +/- 0.57 and 59.7 +/- 1.79 mV concentration decade(-1) and detection limits of 8.91 x 10(-6) and 1.47 x 10(-5) M in case of sibutramine-tetraphenylborate (Sibu-TPB) and sibutramine-phosphotungstate ((Sibu)(3)-PT), respectively. The proposed sensors have been successfully applied for the determination of sibutramine hydrochloride in Regitrim capsules in batch and flow injection (FI) conditions.

  7. Bienzymatic biosensor for rapid detection of aspartame by flow injection analysis.

    Science.gov (United States)

    Radulescu, Maria-Cristina; Bucur, Bogdan; Bucur, Madalina-Petruta; Radu, Gabriel Lucian

    2014-01-09

    A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX), carboxyl esterase (CaE) and bovine serum albumin (BSA) were immobilised with glutaraldehyde (GA) onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC). The biosensor response was fast. The sample throughput using a flow injection analysis (FIA) system was 40 h⁻¹ with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 µM for methanol and 0.2 µM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples) without any pre-treatment step prior to measurement.

  8. Chemiluminescence determination of ultramicro DNA with a flow-injection method

    International Nuclear Information System (INIS)

    Chen Hui; Zhou Min; Jin Xiaoyong; Song Yumin; Zhang Ziyu; Ma Yongjun

    2002-01-01

    A high sensitive flow-injection chemiluminescence method for determination of calf thymus DNA and herring sperm DNA has been developed. The method is based on the chemiluminescence reaction of Rhodamine B-cerium(IV)-thermally denatured DNAs in sulfuric acid media. The proposed procedure allows quantitation of DNAs in the range 2.6x10 -5 to 0.26 μg ml -1 for calf thymus DNA and 5.0x10 -8 to 5.0x10 -5 μg ml -1 for herring sperm DNA with correlation coefficients 0.9998 and 0.9996 (both n=11), respectively. The detection limits (3σ) are 6.5x10 -6 μg ml -1 for calf thymus DNA and 4.3x10 -8 μg ml -1 for herring sperm DNA. The possible mechanism of chemiluminescence in the system is discussed

  9. Determination of uranium in organic phase by flow injection spectrophotometric analysis

    International Nuclear Information System (INIS)

    Yu Yiyun

    1998-01-01

    Based on the use of merging zone circuit and simulating a series of standard solution of uranium in organic phase, uranium in unknown organic phase sample was determined by flow injection spectrophotometry. A linear calibration graph was obtained with correlation coefficient of 0.999 for uranium concentration in organic phase over 10∼200 mg/L. Isopropyl alcohol was used as carrier solution. Mixing colour solution contains isopropyl alcohol, triethanolamine, masking reagent and Br-PADAP. The relative standard deviation of the method was better than +-5%. Determination of each sample can be completed in one minute. The method characteristic is: (1) using merging zone and simulating standard solution of uranium in organic phase, the method is sensitive and reliable; (2) even if the determined solution was in turbid condition, it can be quantitatively determined; (3) by means of solution replace technique, the tube of peristaltic pump can be used over a long period of time

  10. Spectrophotometric determination of uranium and thorium with arsenazo III in the flow injection system

    International Nuclear Information System (INIS)

    Andrade, M. das G.M. de.

    1986-12-01

    A simple system for flow injection analysis (FIA) with double confluence was built using a filter photocolorimeter, an analogic potentiometer, 'plexiglass' flow cuvettes, polyethylene colls and tubes, 'plexiglass' commuter and peristaltic pump to introduce solutions and gravity as flow source. The system was dimensioned and studied using only Arsenazo III solutions. Spectrophotometric methods for uranium and thorium using Arsenazo III were studied using a scanning spectrophotometer and after chosing adequate red filter, adapted to photocolorimetry using flow cuvettes and FIA. Synthetic samples, phosphate rock, and process samples from uranium recovery of dolomites were analysed. Rocks of Morro do Ferro (MG, Brazil), Caldasite (Baddeleyte + Zirconite), Zirconite, Monazite from a program for certification and certified rocks (Dunite DC-1, CANMET) were analysed without chemical separation of Th (IV) and with ion exchange separation in semi-micro columns of cation exchange resin (Dowex 50). (Author) [pt

  11. Espectrofotometria de zinco em fertilizantes em fluxo Flow injection spectrophotometry of zinc in mineral fertilizers

    Directory of Open Access Journals (Sweden)

    Arnaldo Antonio Rodella

    1999-07-01

    Full Text Available Um sistema de análise química por injeção em fluxo é proposto para a determinação espectrofotométrica de zinco em amostras de misturas de fertilizantes minerais, empregando-se zincon como reagente cromogênico. O procedimento analítico envolve redução de íons metálicos por ácido ascórbico, complexação com íon cianeto, seguindo-se a descomplexação seletiva do zinco com formaldeído, liberando-o para que reaja com o zincon formando um complexo azul. A aplicação do método proposto à extratos de mistura de fertilizantes indicou que a ação de interferentes pode ser contornada e que resultados comparáveis aos da espectrometria de absorção atômica são obtidos.A flow injection system for zinc analysis in mineral fertilizer mixtures is proposed using zincon as chromogenic reagent. The effect of interfering ions such as Cu2+, Fe3+, Mn2+ was eliminated by reduction (using ascorbic acid and complexation of these metal íons with cyanide, with zinc included. Zinc is allowed to react with zincon only after the destruction of the zinc cyano complex with formaldehyde. Flow injection analysis permitted efficient control of the reaction time so that only the zinc ion is set free to produce a blue complex with zincon. Zinc was determined in 16 fertilizer mixtures (3 replicates with precision and accuracy comparable to atomic absorption spectrometry.

  12. Use of flow injection mass spectrometric fingerprinting and chemometrics for differentiation of three black cohosh species

    International Nuclear Information System (INIS)

    Huang, Huilian; Sun, Jianghao; McCoy, Joe-Ann; Zhong, Haiyan; Fletcher, Edward J.; Harnly, James; Chen, Pei

    2015-01-01

    Flow injection mass spectrometry (FIMS) was used to provide chemical fingerprints of black cohosh (Actaea racemosa L.) in a manner of minutes by omitting the separation step. This method has proven to be a powerful tool for botanical authentication and in this study it was used to distinguish between three Actaea species prior to a more detailed chemical analysis using ultra high-performance liquid chromatography high-resolution mass spectrometry (UHPLC–HRMS). Black cohosh has become increasingly popular as a dietary supplement in the United States for the treatment of symptoms related to menopause. However, it has been known to be adulterated with the Asian Actaea dahurica (Turcz. ex Fisch. & C.A.Mey.) Franch. species (syn. Cimicifuga dahurica (Turcz.) Maxim). Existing methods for identification of black cohosh and differentiation of Actaea species are usually lengthy, laborious, and lack robustness, often based on the comparison of a few pre-selected components. Chemical fingerprints were obtained for 77 black cohosh samples and their related species using FIMS in the negative ion mode. The analysis time for each sample was less than 2 min. All data were processed using principal component analysis (PCA). FIMS fingerprints could readily differentiate all three species. Representative samples from each of the three species were further examined using UHPLC–MS to provide detailed profiles of the chemical differences between the three species and were compared to the PCA loadings. This study demonstrates a simple, fast, and easy analytical method that can be used to differentiate A. racemosa, Actaea podocarpa, and A. dahurica. - Highlights: • Flow injection mass spectrometry (FIMS) was used to provide chemical fingerprints of black cohosh (Actaea racemosa L.) in a manner of minutes by omitting the separation step. • FIMS can discriminate between A. dahurica, A. podocarpa, and A. racemosa. • FIMS is a valuable screening tool for authentication of botanicals

  13. Use of flow injection mass spectrometric fingerprinting and chemometrics for differentiation of three black cohosh species

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Huilian [Food Composition and Methods Development Laboratory, Beltsville Human Nutrition Research Center, Agricultural Research Service, U.S. Department of Agriculture, Beltsville, MD (United States); Key Laboratory of Modern Preparation of TCM, Jiangxi University of Traditional Chinese Medicine, Ministry of Education, Nanchang, Jiangxi Province (China); Sun, Jianghao [Food Composition and Methods Development Laboratory, Beltsville Human Nutrition Research Center, Agricultural Research Service, U.S. Department of Agriculture, Beltsville, MD (United States); McCoy, Joe-Ann [The North Carolina Arboretum Germplasm Repository, UNC Affiliate Campus, Asheville, NC (United States); Zhong, Haiyan [College of Food Science and Engineering, Central South University of Forestry and Technology, Changsha, Hunan Province (China); Fletcher, Edward J. [Strategic Sourcing, Inc., Banner Elk, NC 28604 (United States); Harnly, James, E-mail: harnly.james@ars.usda.gov [Food Composition and Methods Development Laboratory, Beltsville Human Nutrition Research Center, Agricultural Research Service, U.S. Department of Agriculture, Beltsville, MD (United States); Chen, Pei, E-mail: pei.chen@ars.usda.gov [Food Composition and Methods Development Laboratory, Beltsville Human Nutrition Research Center, Agricultural Research Service, U.S. Department of Agriculture, Beltsville, MD (United States)

    2015-03-01

    Flow injection mass spectrometry (FIMS) was used to provide chemical fingerprints of black cohosh (Actaea racemosa L.) in a manner of minutes by omitting the separation step. This method has proven to be a powerful tool for botanical authentication and in this study it was used to distinguish between three Actaea species prior to a more detailed chemical analysis using ultra high-performance liquid chromatography high-resolution mass spectrometry (UHPLC–HRMS). Black cohosh has become increasingly popular as a dietary supplement in the United States for the treatment of symptoms related to menopause. However, it has been known to be adulterated with the Asian Actaea dahurica (Turcz. ex Fisch. & C.A.Mey.) Franch. species (syn. Cimicifuga dahurica (Turcz.) Maxim). Existing methods for identification of black cohosh and differentiation of Actaea species are usually lengthy, laborious, and lack robustness, often based on the comparison of a few pre-selected components. Chemical fingerprints were obtained for 77 black cohosh samples and their related species using FIMS in the negative ion mode. The analysis time for each sample was less than 2 min. All data were processed using principal component analysis (PCA). FIMS fingerprints could readily differentiate all three species. Representative samples from each of the three species were further examined using UHPLC–MS to provide detailed profiles of the chemical differences between the three species and were compared to the PCA loadings. This study demonstrates a simple, fast, and easy analytical method that can be used to differentiate A. racemosa, Actaea podocarpa, and A. dahurica. - Highlights: • Flow injection mass spectrometry (FIMS) was used to provide chemical fingerprints of black cohosh (Actaea racemosa L.) in a manner of minutes by omitting the separation step. • FIMS can discriminate between A. dahurica, A. podocarpa, and A. racemosa. • FIMS is a valuable screening tool for authentication of botanicals.

  14. Band-type microelectrodes for amperometric immunoassays

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Ga-Yeon; Chang, Young Wook; Ko, Hyuk [Department of Materials Science and Engineering, Yonsei University, 134 Shinchon-dong, Seodaemun-gu, Seoul, 120-749 (Korea, Republic of); Kang, Min-Jung [Korea Institute of Science and Technology (KIST), Seoul (Korea, Republic of); Pyun, Jae-Chul, E-mail: jcpyun@yonsei.ac.kr [Department of Materials Science and Engineering, Yonsei University, 134 Shinchon-dong, Seodaemun-gu, Seoul, 120-749 (Korea, Republic of)

    2016-07-20

    A band-type microelectrode was made using a parylene-N film as a passivation layer. A circular-type, mm-scale electrode with the same diameter as the band-type microelectrode was also made with an electrode area that was 5000 times larger than the band-type microelectrode. By comparing the amperometric signals of 3,5,3′,5′-tetramethylbenzidine (TMB) samples at different optical density (OD) values, the band-type microelectrode was determined to be 9 times more sensitive than the circular-type electrode. The properties of the circular-type and the band-type electrodes (e.g., the shape of their cyclic voltammograms, the type of diffusion layer used, and the diffusion layer thickness per unit electrode area) were characterized according to their electrode area using the COMSOL Multiphysics software. From these simulations, the band-type electrode was estimated to have the conventional microelectrode properties, even when the electrode area was 100 times larger than a conventional circular-type electrode. These results show that both the geometry and the area of an electrode can influence the properties of the electrode. Finally, amperometric analysis based on a band-type electrode was applied to commercial ELISA kits to analyze human hepatitis B surface antigen (hHBsAg) and human immunodeficiency virus (HIV) antibodies. - Highlights: • A band-type microelectrode was made using a parylene-N film as a passivation layer. • The band-type microelectrode was 14-times more sensitive than circular-type electrode. • The influence of geometry on microelectrode properties was simulated using COMSOL. • The band-type electrode was applied to ELISA kits for hHBsAg and hHIV-antibodies.

  15. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Yanlin [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia); Adeloju, Samuel B., E-mail: Sam.Adeloju@monash.edu [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia)

    2012-04-06

    Highlights: Black-Right-Pointing-Pointer Successful speciation of inorganic and organic Hg with Fe{sup 3+}, Cu{sup 2+} and thiourea as catalysts. Black-Right-Pointing-Pointer Best sensitivity enhancement and similar sensitivity for MeHg and Hg{sup 2+} with Fe{sup 3+}. Black-Right-Pointing-Pointer Successful use of Hg{sup 2+} as the primary standard for quantification of inorganic and total-Hg. Black-Right-Pointing-Pointer Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. Black-Right-Pointing-Pointer Integration with FIA for rapid analysis with a sample throughput of 180 h{sup -1}. - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH{sub 4} were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe{sup 3+}, Cu{sup 2+} and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu{sup 2+} and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe{sup 3+} gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg{sup 2+}. Due to similarity of resulting sensitivity, Hg{sup 2+} was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury

  16. Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Zhang Yanlin; Adeloju, Samuel B.

    2012-01-01

    Highlights: ► Successful speciation of inorganic and organic Hg with Fe 3+ , Cu 2+ and thiourea as catalysts. ► Best sensitivity enhancement and similar sensitivity for MeHg and Hg 2+ with Fe 3+ . ► Successful use of Hg 2+ as the primary standard for quantification of inorganic and total-Hg. ► Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. ► Integration with FIA for rapid analysis with a sample throughput of 180 h −1 . - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH 4 were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe 3+ , Cu 2+ and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu 2+ and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe 3+ gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg 2+ . Due to similarity of resulting sensitivity, Hg 2+ was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h −1 .

  17. Comparison of Flow Injection MS, NMR, and DNA Sequencing: Methods for Identification and Authentication of Black Cohosh (Actaea racemosa)

    Science.gov (United States)

    Flow injection mass spectrometry (FIMS) and proton nuclear magnetic resonance spectrometry (1H-NMR), two metabolic fingerprinting methods, and DNA sequencing were used to identify and authenticate Actaea species. Initially, samples of Actaea racemosa L. from a single source were distinguished from ...

  18. Mass spectrometric confirmation criterion for product-ion spectra generated in flow-injection analysis. Environmental application

    NARCIS (Netherlands)

    Geerdink, R.B.; Niessen, W.M.A.; Brinkman, U.A.T.

    2001-01-01

    The suitability of a confirmation criterion recently recommended in the Netherlands for gas chromatography with mass spectrometric detection (GC-MS), was evaluated for flow-injection analysis (FIA) with atmospheric pressure chemical ionisation MS-MS detection. The main feature of the criterion is

  19. Flow injection on-line preconcentration of low levels of Cr(VI) with detection by ETAAS

    DEFF Research Database (Denmark)

    Som-aum, Waraporn; Liawruangrath, Saisunee; Hansen, Elo Harald

    2002-01-01

    A flow injection (FI) on-line sorption preconcentration procedure utilizing a packed column reactor and combined with electrothermal atomic absorption spectrometry (ETAAS) is proposed for the determination of low levels of Cr(VI) in water samples. Polytetrafluoroethylene (PTFE) beads packed in a ...

  20. How Flow Injection Analysis (FIA) over the past 25 years has changed our way of performing chemical analyses

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2007-01-01

    Briefly looking back on the impact of flow injection analysis (FIA), as reflected in the rapid growth of publications in the scientific literature, and touching upon many of the novel and unique analytical chemical possibilities that FIA and its sequels, sequential injection analysis (SIA) and La...

  1. Trends and perspectives of flow injection/sequential injection on-line sample-pretreatment schemes coupled to ETAAS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2005-01-01

    Flow injection (FI) analysis, the first generation of this technique, became in the 1990s supplemented by its second generation, sequential injection (SI), and most recently by the third generation (i.e.,Lab-on-Valve). The dominant role played by FI in automatic, on-line, sample pretreatments in ...

  2. Flow injection methods for the determination of a-tocopherol with spectrophotometric detection

    International Nuclear Information System (INIS)

    Rishi, L.; Waseem, A.; Yaqoob, M.; Nabi, A.; Jadoon, S.

    2011-01-01

    The present paper describes flow injection procedures for a-tocopherol determination in pharmaceuticals and infant milk powder based on spectrophotometric detection. These two procedures are based on the reduction of iron(III) to iron(II) and of Mo(Vi) to Mo(V) by a-tocopherol and subsequent formation of iron(II)-o-phenanthroline, and phospho molybdenum complexes which were monitored at 510 and 695 nm respectively. Calibration graphs were linear over the concentration range of 0.21-43 mu g/mL for iron(III) and 0.25-10 mu g/mL for Mo(Vi) reduction methods respectively. The limits of detection (3s) of 0.05 and 0.1 mu g/mL with sample throughput of 30 and 50/h respectively were obtained. The relative standard deviations of 1.2- 3.8% (n = 4) was achieved in the concentration range studied. The developed methods were applied to pharmaceuticals and infant milk powders and the results obtained were compared with official method and no significant difference between these methods was observed at 95% confidence level. (author)

  3. Flow injection determination of lead and cadmium in hair samples from workers exposed to welding fumes

    International Nuclear Information System (INIS)

    Cespon-Romero, R.M.; Yebra-Biurrun, M.C.

    2007-01-01

    A flow injection procedure involving continuous acid leaching for lead and cadmium determination in hair samples of persons in permanent contact with a polluted workplace environment by flame atomic absorption spectrometry is proposed. Variables such as sonication time, nature and concentration of the acid solution used as leaching solution, leaching temperature, flow-rate of the continuous manifold, leaching solution volume and hair particle size were simultaneously studied by applying a Plackett-Burman design approach. Results showed that nitric acid concentration (leaching solution), leaching temperature and sonication time were statistically significant variables (confidence interval of 95%). These last two variables were finally optimised by using a central composite design. The proposed procedure allowed the determination of cadmium and lead with limits of detection 0.1 and 1.0 μg g -1 , respectively. The accuracy of the developed procedure was evaluated by the analysis of a certified reference material (CRM 397, human hair, from the BCR). The proposed method was applied with satisfactory results to the determination of Cd and Pb in human hair samples of workers exposed to welding fumes

  4. Reverse flow injection spectrophotometric determination of thiram and nabam fungicides in natural water samples

    International Nuclear Information System (INIS)

    Asghar, M.; Yaqoob, M.; Nabi, A.

    2014-01-01

    A reverse flow injection (rFI) spectrophotometric method is reported for determination of thiram and nabam fungicides in natural water samples. The method is based on the reduction of iron(III) in the presence of thiram/nabam in acidic medium at 60 degree C and formation of iron(II)-ferricyanide complex was measured at 790 nm. The limits of detection (3s blank) were 0.01 and 0.05 micro g mL1 for thiram and nabam respectively with a sample throughput of 60 h1. Calibration graphs were linear over the range of 0.02 - 8.0 micro g mL1 (R2 = 0.9999, n = 8) and 0.1 - 30 micro g mL1 (R2 = 0.9982, n = 10) for thiram and nabam with relative standard deviations (RSDs; n = 3) in the range of 0.8 - 1.6% respectively. Experimental parameters and potential interferences were examined. Thiram and nabam were determined in natural water samples using solid-phase extraction (SPE) procedure and recoveries were in the range of 93+-3 - 105+-2% and 87+-4 - 102+-3% respectively. The results obtained were not significantly different compared with a HPLC method. (author)

  5. Chemiluminescence determination of ultramicro DNA with a flow-injection method

    Energy Technology Data Exchange (ETDEWEB)

    Chen Hui; Zhou Min; Jin Xiaoyong; Song Yumin; Zhang Ziyu; Ma Yongjun

    2002-02-12

    A high sensitive flow-injection chemiluminescence method for determination of calf thymus DNA and herring sperm DNA has been developed. The method is based on the chemiluminescence reaction of Rhodamine B-cerium(IV)-thermally denatured DNAs in sulfuric acid media. The proposed procedure allows quantitation of DNAs in the range 2.6x10{sup -5} to 0.26 {mu}g ml{sup -1} for calf thymus DNA and 5.0x10{sup -8} to 5.0x10{sup -5} {mu}g ml{sup -1} for herring sperm DNA with correlation coefficients 0.9998 and 0.9996 (both n=11), respectively. The detection limits (3{sigma}) are 6.5x10{sup -6} {mu}g ml{sup -1} for calf thymus DNA and 4.3x10{sup -8} {mu}g ml{sup -1} for herring sperm DNA. The possible mechanism of chemiluminescence in the system is discussed.

  6. Phenylboronic acid immunoaffinity reactor coupled with flow injection chemiluminescence for determination of {alpha}-fetoprotein

    Energy Technology Data Exchange (ETDEWEB)

    Wu Yafeng [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China); Zhuang Yafeng [Department of Chemistry, Changzhou Institute of Technology, Changzhou 213022 (China); Liu Songqin [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China)], E-mail: liusq@seu.edu.cn; He Lin [Department of Chemistry, North Carolina State University, Raleigh, NC 27695-8204 (United States)

    2008-12-23

    A reusable and sensitive immunoassay based on phenylboronic acid immunoaffinity reactor in combination with flow injection chemiluminescence (CL) for determination of glycoprotein was described. The reactor was fabricated by immobilizing 3-aminophenylboronic acid (APBA) on glass microbeads with {gamma}-glycidoxypropyltrimethoxysilane (GPMS) as linkage. The {alpha}-fetoprotein (AFP) could be easily immobilized on the APBA coated beads through sugar-boronic interaction. After an off-line incubation, the mixture of the analyte AFP with horseradish peroxidase-labeled AFP antibody (HRP-anti-AFP) was injected into the reactor. This led the trapping of free HRP-anti-AFP by the surface coated AFP on glass beads. The trapped HRP-anti-AFP was detected by chemiluminescence due to its sensitizing effect on the reaction of luminol and hydrogen peroxide. Under optimal conditions, the chemiluminescent signal was proportional to AFP concentration in the range of 10-100 ng mL{sup -1}. The whole assay process including regeneration of the reactor could be completed within 31 min. The proposed system showed acceptable detection and fabrication reproducibility, and the results obtained with the present method were in acceptable agreement with those from parallel single-analyte test of practical clinical sera. The described method enabled a low-cost, time saving and was potential to detect the serum AFP level in clinical diagnosis.

  7. Flow injection spectrophotometry using natural reagent from Morinda citrifolia root for determination of aluminium in tea.

    Science.gov (United States)

    Tontrong, Sopa; Khonyoung, Supada; Jakmunee, Jaroon

    2012-05-01

    A flow injection (FI) spectrophotometric method with using natural reagent extracted from Morinda citrifolia root has been developed for determination of aluminium. The extract contained anthraquinone compounds which could react with Al(3+) to form reddish complexes which had maximum absorption wavelength at 499.0nm. The extract could be used as a reagent in FI system without further purification to obtain pure compound. A sensitive method for determination of aluminium in concentration range of 0.1-1.0mgL(-1), with detection limit of 0.05mgL(-1) was achieved. Relative standard deviations of 1.2% and 1.7% were obtained for the determination of 0.1 and 0.6mgL(-1) Al(3+) (n=11). Sample throughput of 35h(-1) was achieved with the consumption of 3mL each of carrier and reagent solutions per injection. The developed method was successfully applied to tea samples, validated by the FAAS standard method. The method is simple, fast, economical and could be classified as a greener analytical method. Copyright © 2011 Elsevier Ltd. All rights reserved.

  8. Screen-printed sensor for batch and flow injection potentiometric chromium(VI) monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Moreno, Raul A.; Gismera, M.J.; Sevilla, M.T.; Procopio, Jesus R. [Facultad de Ciencias, Universidad Autonoma de Madrid, Departamento de Quimica Analitica y Analisis Instrumental, Madrid (Spain)

    2010-05-15

    A disposable screen-printed electrode was designed and evaluated for direct detection of chromium(VI) in batch and flow analysis. The carbon screen-printed electrode was modified with a graphite-epoxy composite. The optimal graphite-epoxy matrix contains 37.5% graphite powder, 12.5% diphenylcarbohydrazide, a selective compound for chromium(VI), and 50% epoxy resin. The principal analytical parameters of the potentiometric response in batch and flow analysis were optimized and calculated. The screen-printed sensor exhibits a response time of 20 {+-} 1 s. In flow analysis, the analytical frequency of sampling is 70 injections per hour using 0.1 M NaNO{sub 3} solution at pH 3 as the carrier, a flow rate of 2.5 mL.min{sup -1}, and an injection sample volume of 0.50 mL. The sensor shows potentiometric responses that are very selective for chromium(VI) ions and optimal detection limits in both static mode (2.1 x 10{sup -7} M) and online analysis (9.4 x 10{sup -7} M). The disposable potentiometric sensor was employed to determine toxicity levels of chromium(VI) in mineral, tap, and river waters by flow-injection potentiometry and batch potentiometry. Chromium(VI) determination was also carried out with successful results in leachates from municipal solid waste landfills. (orig.)

  9. Polyion selective polymeric membrane-based pulstrode as a detector in flow-injection analysis.

    Science.gov (United States)

    Bell-Vlasov, Andrea K; Zajda, Joanna; Eldourghamy, Ayman; Malinowska, Elzbieta; Meyerhoff, Mark E

    2014-04-15

    A method for the detection of polyions using fully reversible polyion selective polymeric membrane type pulstrodes as detectors in a flow-injection analysis (FIA) system is examined. The detection electrode consists of a plasticized polymeric membrane doped with 10 wt % of tridodecylmethylammonium-dinonylnaphthalene sulfonate (TDMA/DNNS) ion-exchanger salt. The pulse sequence used involves a short (1 s) galvanostatic pulse, an open-circuit pulse (0.5 s) during which the EMF of the cell is measured, and a longer (15 s) potentiostatic pulse to return the membrane to its original chemical composition. It is shown that total pulse sequence times can be optimized to yield reproducible real-time detection of injected samples of protamine and heparin at up to 20 samples/h. Further, it is shown that the same membrane detector can be employed for FIA detection of both polycations at levels ≥10 μg/mL and polyanions at levels of ≥40 μg/mL by changing the direction of the galvanostatic pulse. The methodology described may also be applicable in the detection of polyionic species at low levels in other flowing configurations, such as in liquid chromatography and capillary electrophoresis.

  10. A multisyringe flow injection method for the determination of thorium in water samples using spectrophotometric detection

    International Nuclear Information System (INIS)

    Guzman-Mar, J.L.; Aracely Hernandez-Ramirez; Lopez-Chuken, U.J.; Lopez-de-Alba, P.L.; Victor Cerda

    2011-01-01

    A fast and simple multisyringe flow injection analysis (MSFIA) method for routine determination of thorium in water samples was developed. The methodology was based on the complexation reaction of thorium with arsenazo (III) at pH 2.0. Thorium concentrations were spectrophotometrically detected at 665 nm. Under optimal conditions, Beer's law was obeyed over the range from 0.2 to 4.5 μg mL -1 thorium, a 3σ detection limit of 0.05 μg mL -1 , and a 10σ quantification limit of 0.2 μg mL -1 were obtained. The relative standard deviations (RSD, %) at 0.5, 2.5 and 4.5 μg mL -1 was 2.8, 1.5 and 0.8%, respectively (n = 10). It was found that most of the common metal ions and anions did not interfere with the thorium determination. The proposed method was successfully applied to its analysis in various water samples. (author)

  11. Stopped-flow injection spectrophotometric method for determination of chlorate in soil

    Directory of Open Access Journals (Sweden)

    Jaroon Jakmunee

    2008-06-01

    Full Text Available A stopped-flow injection (FI spectrophotometric procedure based on iodometric reaction for the determination of chlorate has been developed. Standard/sample was injected into a stream of potassium iodide solution and then merged with a stream of hydrochloric acid solution to produce triiodide. By stopping the flow while the sample zone is being in a mixing coil, a slow reaction of chlorate with iodide in acidic medium was promoted to proceed with minimal dispersion of the triiodide product zone. When the flow started again, a concentrated product zone was pushed into a flow cell and a signal profile due to light absorption of the product was recorded. Employing a lab-built semi-automatic stopped-FI analyser, the analysis can be performed with higher degree of automation and low chemical consumption. Linear calibration graph in the range of 5-50 mg ClO3- L-1 was obtained, with detection limit of 1.4 mg ClO3- L-1. Relative standard deviation of 2.2% (30 mg ClO3- L-1, n=10 and sample throughput of about 20 h-1 were achieved. The system was applied to soil samples and validated by batch spectrophotometric and standard titrimetric methods.

  12. Evaluation of Antibacterial Enrofloxacin in Eggs by Matrix Solid Phase Dispersion-Flow Injection Chemiluminescence

    Directory of Open Access Journals (Sweden)

    Xiaocui Duan

    2014-01-01

    Full Text Available The study based on the chemiluminescence (CL reaction of potassium ferricyanide and luminol in sodium hydroxide medium, enrofloxacin (ENRO could dramatically enhance CL intensities and incorporated with matrix solid-phase dispersion (MSPD technique (Florisil used as dispersant, dichloromethane eluted the target compounds. A simple flow injection chemiluminescence (FL-CL method with MSPD technique for determination of ENRO in eggs was described. Under optimal conditions, the CL intensities were linearly related to ENRO concentration ranging from 4.0×10-8 g.L−1 to 5.0×10-5 g.L−1, with a correlation coefficient of 0.9989 and detection limit of 5.0×10-9 g.L−1. The relative standard deviation was 3.6% at an ENRO concentration of 2.0×10-6 g.L−1. Our testing technique can help ensure food safety, and thus, protect public health.

  13. Determination of Nitrite and Nitrate in Natural Waters Using Flow Injection with Spectrophotometric Detection

    International Nuclear Information System (INIS)

    Yaqoob, M.; Nabi, A.

    2013-01-01

    A simple and sensitive flow injection spectrophotometric method is reported for the room temperature determination of nitrite and nitrate based on the Griess reaction and a copperised cadmium column for reduction of nitrate. Calibration graphs were linear over the range 2 - 1000 micro g N L /sup -1/ (R2 = 0.9997 and 0.9999, n = 9) with a limit of detection (3 s.d.) of 1.0 micro g N L and relative standard deviations (n = 10) of 0.9 and 1.2% for 50 micro g N L nitrite and nitrate respectively. The sample throughput was 50 h. The effect of reagent concentrations, physical parameters (flow rate, sample volume, reaction coil and copperised cadmium column length) and the potential interferences are reported. The effect of salinity on the blank and on the determination of nitrite and nitrate are also presented. The method was applied to natural waters (rainwater, freshwater and estuarine water) and the results for nitrite + nitrate (140 - 7310 micro g N L/sup -1/) were not significantly different (95% confidence interval) from results obtained using a segmented flow analyser reference method with spectrophotometric detection. (author)

  14. Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Leal, L.O.; Elsholz, O.; Forteza, R.; Cerda, V.

    2006-01-01

    A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl 2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L -1 . The detection limit (3σ b /S) achieved is 5 ng L -1 . The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L -1 Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples

  15. Stopped-flow injection method for determination of phosphate in soils and fertilisers

    Directory of Open Access Journals (Sweden)

    Jaroon Jakmunee

    2008-02-01

    Full Text Available A stopped-flow injection system for the determination of phosphate has been developed. It involves the phosphate-molybdate-ascorbic acid reactions in the molybdenum blue method. The system is controlled by a semi-automatic stopped-FI analyser with a light emitting diode (LED-colorimeter for monitoring the absorbance change relating to the concentration of a reaction product formed during the stopping period while the injected zone of a standard or sample is being in the flow cell. The slope of the FIAgram obtained is linearly proportional to the reaction rate, which depends on the phosphate concentration. Effects of concentration of reagents, viz. sodium molybdate, ascorbic acid and nitric acid, on the slope of the FIAgram were studied. The suitable concentration is 0.02 M, 0.25 %w/v and 0.15 M, respectively. A linear calibration graph in the range of 0.3-6.0 mg P L-1 was employed for the determination of phosphate in soil and fertiliser samples. The results obtained agree well with those from a standard spectrophotometric method.

  16. [Research on optimization of mathematical model of flow injection-hydride generation-atomic fluorescence spectrometry].

    Science.gov (United States)

    Cui, Jian; Zhao, Xue-Hong; Wang, Yan; Xiao, Ya-Bing; Jiang, Xue-Hui; Dai, Li

    2014-01-01

    Flow injection-hydride generation-atomic fluorescence spectrometry was a widely used method in the industries of health, environmental, geological and metallurgical fields for the merit of high sensitivity, wide measurement range and fast analytical speed. However, optimization of this method was too difficult as there exist so many parameters affecting the sensitivity and broadening. Generally, the optimal conditions were sought through several experiments. The present paper proposed a mathematical model between the parameters and sensitivity/broadening coefficients using the law of conservation of mass according to the characteristics of hydride chemical reaction and the composition of the system, which was proved to be accurate as comparing the theoretical simulation and experimental results through the test of arsanilic acid standard solution. Finally, this paper has put a relation map between the parameters and sensitivity/broadening coefficients, and summarized that GLS volume, carrier solution flow rate and sample loop volume were the most factors affecting sensitivity and broadening coefficients. Optimizing these three factors with this relation map, the relative sensitivity was advanced by 2.9 times and relative broadening was reduced by 0.76 times. This model can provide a theoretical guidance for the optimization of the experimental conditions.

  17. Study on the interaction of catalase with pesticides by flow injection chemiluminescence and molecular docking.

    Science.gov (United States)

    Tan, Xijuan; Wang, Zhuming; Chen, Donghua; Luo, Kai; Xiong, Xunyu; Song, Zhenghua

    2014-08-01

    The interaction mechanisms of catalase (CAT) with pesticides (including organophosphates: disulfoton, isofenphos-methyl, malathion, isocarbophos, dimethoate, dipterex, methamidophos and acephate; carbamates: carbaryl and methomyl; pyrethroids: fenvalerate and deltamethrin) were first investigated by flow injection (FI) chemiluminescence (CL) analysis and molecular docking. By homemade FI-CL model of lg[(I0-I)/I]=lgK+nlg[D], it was found that the binding processes of pesticides to CAT were spontaneous with the apparent binding constants K of 10(3)-10(5) L mol(-1) and the numbers of binding sites about 1.0. The binding abilities of pesticides to CAT followed the order: fenvalerate>deltamethrin>disulfoton>isofenphos-methyl>carbaryl>malathion>isocarbophos>dimethoate>dipterex>acephate>methomyl>methamidophos, which was generally similar to the order of determination sensitivity of pesticides. The thermodynamic parameters revealed that CAT bound with hydrophobic pesticides by hydrophobic interaction force, and with hydrophilic pesticides by hydrogen bond and van der Waals force. The pesticides to CAT molecular docking study showed that pesticides could enter into the cavity locating among the four subdomains of CAT, giving the specific amino acid residues and hydrogen bonds involved in CAT-pesticides interaction. It was also found that the lgK values of pesticides to CAT increased regularly with increasing lgP, Mr, MR and MV, suggesting that the hydrophobicity and steric property of pesticide played essential roles in its binding to CAT. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Trace and ultratrace analysis methods for the determination of phosphorus by flow-injection techniques.

    Science.gov (United States)

    Motomizu, Shoji; Li, Zhen-Hai

    2005-04-15

    Trace (phosphorus determination by flow-injection analysis are reviewed. Most of the methods cited in this review are fundamentally based on the reaction of orthophosphate with molybdate to form heteropoly acids, such as molybdenum yellow and molybdenum blue, and some of the methods are based on the formation of such secondary reactions as ion associates and their aggregates with bulky cations, such as cationic dyes and quaternary ammonium ions. The heteropoly acids themselves can be measured by spectrophotometry, and the ion associate formed with a cationic dye, Malachite Green (MG), can be measured based on the coloration of MG. Light scattering detection methods can be used for measuring the aggregates of ion associates formed with bulky cations. Highly sensitive detection of phosphorus can be accomplished by fluorophotometry; Rhodamine B (RB) and its analogues react with molybdophosphate to form ion associates, which shows fluorescence quenching of RB: LOD is about 5 nM. The detection method based on the chemiluminescence of luminal oxidized with molybdophosphoric acids is probably the most sensitive of all the detection methods reported so far: LOD of the method is as low as 1nM. The LOD of the molybdenum blue method can be improved by using a liquid core waveguide: LOD is 0.5 nM.

  19. Batch and flow-injection methods for the spectrophotometric determination of olanzapine

    Energy Technology Data Exchange (ETDEWEB)

    Jasinska, A.; Nalewajko, E

    2004-04-22

    An indirect batch spectrophotometric and direct flow-injection (FI) visible spectrophotometric methods have been developed for the determination of the novel anti-psychotic drug olanzapine (OLA). The batch method is based on the oxidation of olanzapine by a known excess of potassium hexacyanoferrate(III) in the presence of the mixture of sulphuric and phosphoric acids (1:1 (v/v)). The absorbance of unreacted oxidant is measured at 425 nm. The absorbance decreases linearly with increasing concentration of the assayed drug. The FI method with detection at 540 nm is based on the direct oxidation of olanzapine one of two oxidants, cerium(IV) sulphate or potassium hexacyanoferrate(III) in acidic medium. The calibration graph were linear over the range of 2.5-40 {mu}g ml{sup -1} in the batch method and 0.05-300 and 0.5-250 {mu}g ml{sup -1} in the FI methods, used cerium (IV) sulphate and potassium hexacyanoferrate (III) respectively. Both FI methods gave similar results in terms of precision and accuracy. The relative standard deviation (R.S.D.), was <1%. The accuracy, obtained from recovery experiments, was 97.9-99.4%. The batch method gave slightly higher R.S.D. values (up to 2.3%) and lower values of accuracy (the recovery was between 96.5 and 96.6%). The methods developed were applied to the determination of olanzapine in a pharmaceutical product.

  20. Spectrophotometric determination of phosphorus in iron alloys employing a flow injection system

    Directory of Open Access Journals (Sweden)

    Gervasio Ana P. G.

    2001-01-01

    Full Text Available A flow-injection procedure for spectrophotometric determination of phosphorus in electrolytic iron and iron alloys is proposed. The method is based on the ammonium molybdate reaction followed by stannous chloride reduction in acidic medium. In order to circumvent the severe interference caused by the major constituents such as Fe(III and Cr(III, a mini-column packed with AG50W-X8 resin was coupled to the manifold. A sample throughput of 40 determinations per hour, a dynamical range from P 0.25 to 6.00 mg L-1, a reagent consumption of 25 mg ammonium molybdate and 2 mg stannous chloride per determination, and a relative standard deviation < 1% (n = 10 for a typical sample with 2.20 mg L-1 P were achieved. Three different types of samples were used to evaluate system performance. Accuracy was assessed by comparing the results with certified values and no significant difference at 95 % confidence level was observed.

  1. Review of recent applications of flow injection spectrophotometry to pharmaceutical analysis

    International Nuclear Information System (INIS)

    Tzanavaras, Paraskevas D.; Themelis, Demetrius G.

    2007-01-01

    Pharmaceutical analysis is one of the most important fields in analytical chemistry. The discovery of new drugs and the on-going update of international regulations for the safety and efficacy of pharmaceutical formulations demand the continuous development of new analytical methods. Inevitably, automation plays an important role, especially when a lot of samples have to be analyzed in the minimum of time. The present study reviews the applications of flow injection (FI) spectrophotometry to the determination of active pharmaceutical ingredients (APIs) in their respective formulations. However, the topic covered in this study is important not only to pharmaceutical analytical scientists. The principles, figures of merit and 'chemistry' of the presented methods can be of interest to bio-analytical and clinical chemists as well for the analysis of biological samples, to environmental analysts that study the up-to-date demand of the determination of the fate of pharmaceuticals in the environment and even to toxicologists and forensic scientists. This review covers scientific contributions published later than 2000. A variety of FI procedures based on homogeneous (direct UV measurements, colour-forming reactions, metal-drug interactions) and heterogeneous (optical sensors and solid-phase reactors) systems are discussed. A third section covers on-line sample pretreatment (solid-phase extraction, liquid-liquid extraction, on-line digestion, etc.)

  2. Development of nanobody-based flow injection chemiluminescence immunoassay for sensitive detection of human prealbumin.

    Science.gov (United States)

    Ma, Lei; Sun, Yanyan; Kang, Xuejun; Wan, Yakun

    2014-11-15

    Nanobodies, derived from camelid heavy-chain antibodies, have novel and impactful applications in clinical diagnostics. Our objective is to develop a nanobody-based chemiluminescence immunoassay for sensitive detection of human prealbumin (PA). In this context, a phage display nanobody library is constructed via immunizing dromedary camel with human prealbumin. Three nanobodies have been identified by five successive bio-panning steps. Based on their high expression level and good affinity, two out of three are chosen for further study. Magnetic beads (MBs) were functionalized with PEI by acylamide bond formed between the carboxyl group on the surface of the MB. Then, an anti-PA nanobody (Nb1) can be effectively immobilized onto the surface of the functionalized MB using glutaradehyde as the link. The modified MBs with Nb1 can specifically capture the target PA and reacted with silica nanoparticles with co-immobilized HRP and anti-PA nanobody (Nb2). The concentration of PA was detected by flow injection chemiluminescence. When using MB/PEI as the carrier of anti-PA Nb1, the CL signal significantly increased to 4-fold compared with the signal using MB without PEI modification. The CL signal was further amplified to 5-fold when Si/Nb2 was used as the signal probe. Under optimized conditions, the present immunoassay exhibited a wide quantitative range from 0.05 to 1000 μg L(-1) with a detection limit of 0.01 μg L(-1). The sensitivity of the proposed immunoassay offers great promises in providing a sensitive, specific, time saving, and potential method for detecting PA in clinical settings. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Determination of gallic acid with rhodanine by reverse flow injection analysis using simplex optimization.

    Science.gov (United States)

    Phakthong, Wilaiwan; Liawruangrath, Boonsom; Liawruangrath, Saisunee

    2014-12-01

    A reversed flow injection (rFI) system was designed and constructed for gallic acid determination. Gallic acid was determined based on the formation of chromogen between gallic acid and rhodanine, resulting in a colored product with a λmax at 520 nm. The optimum conditions for determining gallic acid were also investigated. Optimizations of the experimental conditions were carried out based on the so-call univariate method. The conditions obtained were 0.6% (w/v) rhodanine, 70% (v/v) ethanol, 0.9 mol L(-1) NaOH, 2.0 mL min(-1) flow rate, 75 μL injection loop and 600 cm mixing tubing length, respectively. Comparative optimizations of the experimental conditions were also carried out by multivariate or simplex optimization method. The conditions obtained were 1.2% (w/v) rhodanine, 70% (v/v) ethanol, 1.2 mol L(-1) NaOH, flow rate 2.5 mL min(-1), 75 μL injection loop and 600 cm mixing tubing length, respectively. It was found that the optimum conditions obtained by the former optimization method were mostly similar to those obtained by the latter method. The linear relationship between peak height and the concentration of gallic acid was obtained over the range of 0.1-35.0 mg L(-1) with the detection limit 0.081 mg L(-1). The relative standard deviations were found to be in the ranges 0.46-1.96% for 1, 10, 30 mg L(-1) of gallic acid (n=11). The method has the advantages of simplicity extremely high selectivity and high precision. The proposed method was successfully applied to the determination of gallic acid in longan samples without interferent effects from other common phenolic compounds that might be present in the longan samples collected in northern Thailand. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Flow injection spectrophotometric determination of Fe(III) and V(v)

    International Nuclear Information System (INIS)

    Elrahman, Azza Mohamed

    2000-01-01

    Phenylflourone was synthesized with the objective of developing a method for determining Fe(III) and V(V) in the pressence of micelles using flow injectoin technique. Phenylflourone showed a wavelength of maximum absorption at 412 nm which was not affected by the presence of miccelles i.e. n-hexadodecylpyridinum bromide and sodium n-dodecylsulphate, but they have different effects on the absorbance of PHF. The example of PHF-Fe(III) and PHF-V(V) showed the wavelength of the maximum absorption at 4428 nm and 412 nm, respectively. Presence of micelles shifted the wavelength of the two complexes to a lower one. Generally the addition of micelles increased the absorbance of phenylflourone metal ions complexes except for PHF-V(V) with hexadodecylpyridinum bromide. With flow injection technique two approaches were practiced the use of micelle as a carrier or water as a carrier. Sodium n-dodecylsulphate increased the absorbance of the two complexes when it was used as a carrier or added to the metal ions using water as carrier. On the other hand, the use of n-hexadodecylpyridinum bromide as carrieer increased the absorbance of the complexes but it decreased the absorbance when it was used in conjunction with metal ions and water as a carrier. After establishing the optimum FI conditions for PHF-Fe(III) and PHF-V(V) complexes, the calibration curves were construction and produced semiliner response in the concentration range studied. Ti(IV) III, Mo(VI) showed a positive interference in PHF-Fe(III) and PHF-V(V) complexes, respectively.(Author)

  5. An electrochemiluminescence-based fibre optic biosensor for choline flow injection analysis.

    Science.gov (United States)

    Tsafack, V C; Marquette, C A; Leca, B; Blum, L J

    2000-01-01

    A fibre optic biosensor based on luminol electrochemiluminescence (ECL) integrated in a flow injection analysis (FIA) system was developed for the detection of choline. The electrochemiluminescence of luminol was generated by a glassy carbon electrode polarised at +425 mV vs. a platinum pseudo-reference electrode. Choline oxidase (Chx) was immobilised either covalently on polyamide (ABC type) or on UltraBind preactivated membranes, or by physical entrapment in a photo-cross-linkable poly(vinyl alcohol) polymer (PVA-SbQ) alone or after absorption on a weak anion exchanger, DEAE (diethylaminoethyl) Sepharose. The optimisation of the reaction conditions and physicochemical parameters influencing the FIA biosensor response demonstrated that the choline biosensor exhibited the best performances in a 30 mM veronal buffer containing 30 mM KCl and 1.5 mM MgCl2, at pH 9. The use of a 0.5 ml min-1 flow rate enabled the measurement of choline by the membrane-based ECL biosensors in 8 or 5 min, with ABC or UltraBind membranes, respectively, whereas the measurement required only 3 min with the DEAE-PVA system. For comparison, the detection of choline was performed with Chx immobilised using the four different supports. The best performances were obtained with the DEAE-PVA-Chx sensing layer, which allowed a detection limit of 10 pmol, whereas with the ABC, the UltraBind and the PVA systems, the detection limits were 300 pmol, 75 pmol and 220 pmol, respectively. The DEAE-based system also exhibited a good operational stability since 160 repeated measurements of 3 nmol of choline could be performed with an RSD of 4.5% whereas the stability under the best conditions was 45 assays with the other supports.

  6. Flow injection chemiluminescence determination of loxoprofen and naproxen with the acidic permanganate-sulfite system

    Directory of Open Access Journals (Sweden)

    Li-Juan Wang

    2011-02-01

    Full Text Available A novel flow injection chemiluminescence (CL method for the determination of loxoprofen and naproxen was proposed based on the CL system of KMnO4, and Na2SO3 in acid media. The CL intensity of KMnO4-Na2SO3 was greatly enhaneed in the presence of loxoprofen and naproxen. The mechanism of the CL reaction was studied by the kinetic proecss and UV-vis absorption and the conditions were optimized. Under optimized conditions, the CL intensity was linear with loxoprofen and naproxen concentration in the range of 7.0 × 10−8 – 1.0 × 10−5 g/mL and 2.0 × 10−7 – 4.0 × 10−6 g/mL with the detection limit of 2.0 × 10−8 g/mL and 3.0 × 10−8 g/mL (S/N = 3, respectively. Thc relative standard deviations were 2.39% and 1.37% for 5.0 × 10−7 g/mL naproxen and 5.0 × 10−7 g/mL loxoprofen (n = 10, respectively. The proposed method was satisfactorily applied to thc determination of loxoprofen and naproxen in pharmaceutical preparations. Keywords: chemiluminescence, KMnO4, loxoprofen, naproxen

  7. Development of an automated flow injection analysis system for determination of phosphate in nutrient solutions.

    Science.gov (United States)

    Karadağ, Sevinç; Görüşük, Emine M; Çetinkaya, Ebru; Deveci, Seda; Dönmez, Koray B; Uncuoğlu, Emre; Doğu, Mustafa

    2018-01-25

    A fully automated flow injection analysis (FIA) system was developed for determination of phosphate ion in nutrient solutions. This newly developed FIA system is a portable, rapid and sensitive measuring instrument that allows on-line analysis and monitoring of phosphate ion concentration in nutrient solutions. The molybdenum blue method, which is widely used in FIA phosphate analysis, was adapted to the developed FIA system. The method is based on the formation of ammonium Mo(VI) ion by reaction of ammonium molybdate with the phosphate ion present in the medium. The Mo(VI) ion then reacts with ascorbic acid and is reduced to the spectrometrically measurable Mo(V) ion. New software specific for flow analysis was developed in the LabVIEW development environment to control all the components of the FIA system. The important factors affecting the analytical signal were identified as reagent flow rate, injection volume and post-injection flow path length, and they were optimized using Box-Behnken experimental design and response surface methodology. The optimum point for the maximum analytical signal was calculated as 0.50 mL min -1 reagent flow rate, 100 µL sample injection volume and 60 cm post-injection flow path length. The proposed FIA system had a sampling frequency of 100 samples per hour over a linear working range of 3-100 mg L -1 (R 2  = 0.9995). The relative standard deviation (RSD) was 1.09% and the limit of detection (LOD) was 0.34 mg L -1 . Various nutrient solutions from a tomato-growing hydroponic greenhouse were analyzed with the developed FIA system and the results were found to be in good agreement with vanadomolybdate chemical method findings. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

  8. Amperometric Bioelectronic Tongue for glucose determination

    Directory of Open Access Journals (Sweden)

    Yazan Al-Issa

    2015-03-01

    Full Text Available An amperometric Bioelectronic Tongue is reported for glucose determination that contains eight sensor electrodes constructed using different metal electrodes (Pt, Au, oxidoreductase enzymes (glucose oxidase, ascorbate oxidase, uricase, and membrane coatings (Nafion, chitosan. The response to varying concentrations of glucose, ascorbic acid, uric acid, and acetaminophen was tested for two models, concentration determination by current density measurements at individual electrodes and concentration determination by a linear regression model for the entire electrode array. The reduced chi-squared for the full array model was found to be about one order of magnitude lower than that for the individual-electrode model. Discrimination of glucose from chemical interference by the other three species is accomplished through a combination of enzyme catalysis, metal electrocatalysis, and membrane surface charge. The benefit of incorporating enzyme electrodes into the sensor array is illustrated by the lower correlation coefficients between different enzyme electrodes relative to non-enzyme coated electrodes. This approach can be more generally applied to detection of other substrates of oxidoreductase enzymes.

  9. A microfabricated electroosmotic pump coupled to a gas-diffusion microchip for flow injection analysis of ammonia

    International Nuclear Information System (INIS)

    Zhu, Zaifang; Lu, Joann J.; Liu, Shaorong; Almeida, M. Inês G. S.; Kolev, Spas D.; Pu, Qiaosheng

    2015-01-01

    We have microfabricated two functional components toward developing a microchip flow injection analysis (FIA) system, i.e., an open-channel electroosmotic pump and a gas-diffusion chip, consisting of two microfabricated glass wafers and a porous polytetrafluoroethylene membrane. This is the first application of gas-diffusion separation in a microchip FIA system. To demonstrate the feasibility of using these two components for performing gas-diffusion FIA, we have incorporated them together with a regular FIA injection valve and a capillary electrophoresis absorbance detector in a flow injection system for determination of ammonia in environmental water samples. This system has a limit of detection of 0.10 mg L −1 NH 3 , with a good repeatability (relative standard deviation of less than 5 % for 4.0 mg L −1 NH 3 ). Parameters affecting its performance are also discussed. (author)

  10. A dilute-and-shoot flow-injection tandem mass spectrometry method for quantification of phenobarbital in urine.

    Science.gov (United States)

    Alagandula, Ravali; Zhou, Xiang; Guo, Baochuan

    2017-01-15

    Liquid chromatography/tandem mass spectrometry (LC/MS/MS) is the gold standard of urine drug testing. However, current LC-based methods are time consuming, limiting the throughput of MS-based testing and increasing the cost. This is particularly problematic for quantification of drugs such as phenobarbital, which is often analyzed in a separate run because they must be negatively ionized. This study examined the feasibility of using a dilute-and-shoot flow-injection method without LC separation to quantify drugs with phenobarbital as a model system. Briefly, a urine sample containing phenobarbital was first diluted by 10 times, followed by flow injection of the diluted sample to mass spectrometer. Quantification and detection of phenobarbital were achieved by an electrospray negative ionization MS/MS system operated in the multiple reaction monitoring (MRM) mode with the stable-isotope-labeled drug as internal standard. The dilute-and-shoot flow-injection method developed was linear with a dynamic range of 50-2000 ng/mL of phenobarbital and correlation coefficient > 0.9996. The coefficients of variation and relative errors for intra- and inter-assays at four quality control (QC) levels (50, 125, 445 and 1600 ng/mL) were 3.0% and 5.0%, respectively. The total run time to quantify one sample was 2 min, and the sensitivity and specificity of the method did not deteriorate even after 1200 consecutive injections. Our method can accurately and robustly quantify phenobarbital in urine without LC separation. Because of its 2 min run time, the method can process 720 samples per day. This feasibility study shows that the dilute-and-shoot flow-injection method can be a general way for fast analysis of drugs in urine. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  11. A new amperometric glucose biosensor based on screen printed carbon electrodes with rhenium(IV - oxide as a mediator

    Directory of Open Access Journals (Sweden)

    ALBANA VESELI

    2012-11-01

    Full Text Available Rhenium(IV-oxide, ReO2, was used as a mediator for carbon paste (CPE and screen printed carbon (SPCE electrodes for the catalytic amperometric determination of hydro-gen peroxide, whose overpotential for the reduction could be lowered to -0.1 V vs. Ag/AgCl in flow injection analysis (FIA using phosphate buffer (0.1 M, pH=7.5 as a carrier. For hydrogen peroxide a detection limit (3σ of 0.8 mg L-1 could be obtained.ReO2-modified SPCEs were used to design biosensors with a template enzyme, i.e. glucose oxidase, entrapped in a Nafion membrane. The resulting glucose sensor showed a linear dynamic range up to 200 mg L-1 glucose with a detection limit (3σ of 0.6 mg L-1. The repeatability was 2.1 % RSD (n = 5 measurements, the reproducibility 5.4 % (n = 5 sensors. The sensor could be applied for the determination of glucose in blood serum in good agreement with a reference method.

  12. Analysis of total polyphenols in wines by FIA with highly stable amperometric detection using carbon nanotube-modified electrodes.

    Science.gov (United States)

    Arribas, Alberto Sánchez; Martínez-Fernández, Marta; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2013-02-15

    The use of glassy carbon electrodes (GCEs) modified with multi-walled carbon nanotube (CNT) films for the continuous monitoring of polyphenols in flow systems has been examined. The performance of these modified electrodes was evaluated and compared to bare GCE by cyclic voltammetry experiments and by flow injection analysis (FIA) with amperometric detection monitoring the response of gallic, caffeic, ferulic and p-coumaric acids in 0.050 M acetate buffer pH 4.5 containing 100 mM NaCl. The GCE modified with CNT dispersions in polyethyleneimine (PEI) provided lower overpotentials, higher sensitivity and much higher signal stability under a dynamic regime than bare GCEs. These properties allowed the estimation of the total polyphenol content in red and white wines with a remarkable long-term stability in the measurements despite the presence of potential fouling substances in the wine matrix. In addition, the versatility of the electrochemical methodology allowed the selective estimation of the easily oxidisable polyphenol fraction as well as the total polyphenol content just by tuning the detection potential at +0.30 or 0.70 V, respectively. The significance of the electrochemical results was demonstrated through correlation studies with the results obtained with conventional spectrophotometric assays for polyphenols (Folin-Ciocalteu, absorbance at 280 nm index and colour intensity index). Copyright © 2012 Elsevier Ltd. All rights reserved.

  13. Non-enzymatic amperometric sensor for hydrogen peroxide based on a biocomposite made from chitosan, hemoglobin, and silver nanoparticles

    International Nuclear Information System (INIS)

    Tian, L.; Feng, Y.; Qi, Y.; Wang, B.; Chen, Y.; Fu, X.

    2012-01-01

    We report on a novel non-enzymatic sensor for hydrogen peroxide (HP) that is based on a biocomposite made up from chitosan (CS), hemoglobin (Hb), and silver nanoparticles (AgNPs). The AgNPs were prepared in the presence of CS and glucose in an ultrasonic bath, and CS is found to act as a stabilizing agent. They were then combined with Hb and CS to construct a carbon paste biosensor. The resulting electrode gave a well-defined redox couple for Hb, with a formal potential of about -0.17 V (vs. SCE) at pH 6. 86 and exhibited a remarkable electrocatalytic activity for the reduction of HP. The sensor was used to detect HP by flow injection analysis, and a linear response is obtained in the 0. 08 to 250 μM concentration range. The detection limit is 0.05 μM (at S/N = 3). These characteristics, along with its long-term stability make the sensor highly promising for the amperometric determination of HP. (author)

  14. Amperometric and coulometric methods of platinum metal determination. (Review)

    International Nuclear Information System (INIS)

    Ezerskaya, N.A.

    1981-01-01

    Reviewed are works published in the period from 1957-1979, on amperometric and coulometric (potentiostatistic and amperostatistic variant) determination of platinum metals, Ru in particular. During amperometric titration of Ru the following titrantes are used: hydroquinone, thioxne thiourea, Na 2 S 2 O 3 . It is proposed to titrate Ru in the form of ruthenate-ion with hydrazine sulphate in alkal: medium according to the current of reagent oxidation. During coulometric determination of Ru the electrogenerating titrant TiCl 3 or Ti 2 (SO 4 ) 3 (for initial form of Ru [RuCl 6 ] 2- ) is used [ru

  15. A multisyringe flow injection system with immobilized glucose oxidase based on homogeneous chemiluminescence detection

    International Nuclear Information System (INIS)

    Manera, Matias; Miro, Manuel; Estela, Jose Manuel; Cerda, Victor

    2004-01-01

    In this paper, enzyme containing reactors are for the first time implemented in the multisyringe flow injection analysis (MSFIA) technique interfaced with chemiluminescence detection for biochemical assays. The automated methodology is based on the on-line substrate conversion in an oxidase packed-bed reactor and the post-column chemiluminogenic catalysed-reaction of the generated oxidising species with an organic molecule (namely, 3-aminophthalhydrazide) in front of the photosensor module. Various catalysts in homogeneous phase are compared taking advantage of the benefits of the MSFIA concept. On one hand, mineral catalysts (namely, Co(II)) are assessed, on the other hand, minute and accurate volumes of soluble organic species (viz., horseradish peroxidase (HRP)) are readily handled without requiring further immobilization protocols. The potentials of the MSFIA-CL concept with immobilisation of the proper oxidase protein are demonstrated using glucose as a model of substrate. Despite the different pH and kinetic requirements for both the substrate conversion in the enzyme-reactor and the Co(II)/HRP-mediated luminol oxidation integrated in the flow system, the MSFIA approach warrants maximum yields owing to the independent optimisation of the physical and chemical parameters of the various reactions involved. Under the optimised configurations and experimental variables, dynamic working ranges from 2.5x10 -6 to 1.0x10 -3 mol l -1 glucose may be obtained for both detection schemes by proper photomultiplier gain selection. The detection and determination limits calculated at the 3σ and 10σ level were 8.6x10 -7 and 2.0x10 -6 mol l -1 glucose, respectively, for the Co(II)-luminol system, and 1.3x10 -6 and 2.3x10 -6 mol l -1 glucose, respectively, for the HRP-luminol procedure. The repeatability (n=10) at the 1.0x10 -5 mol l -1 level was slightly better for the Co(II)-catalysed reaction (2.5% versus 4.0%). The developed MSFIA-CL methodology was used for kinetic

  16. Amperometric Carbon Fiber Nitrite Microsensor for In Situ Biofilm Monitoring

    Science.gov (United States)

    A highly selective needle type solid state amperometric nitrite microsensor based on direct nitrite oxidation on carbon fiber was developed using a simplified fabrication method. The microsensor’s tip diameter was approximately 7 µm, providing a high spatial resolution of at lea...

  17. Flow-injection fluorimetric determination of menadione using on-line photo-reduction in micellar media

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Ruiz, Tomas; Martinez-Lozano, Carmen; Tomas, Virginia; Martin, Jesus

    2004-07-01

    A very sensitive fluorimetric method for the determination of menadione using a flow injection system is proposed. The method is based on the on-line reduction of menadione in dodecylsulphate micelles upon irradiation with UV light. The strong fluorescence of the reduced menadione in micellar medium is measured at 410 nm with excitation at 340 nm. The method shows a linear range between 2.42 and 245 ng ml{sup -1} and a limit of detection of 0.18 ng ml{sup -1}. The sample throughput was 90 injections per hour. The applicability of the assay was demonstrated by analysing this vitamin in commercial pharmaceutical preparations.

  18. Flow-injection fluorimetric determination of menadione using on-line photo-reduction in micellar media

    International Nuclear Information System (INIS)

    Perez-Ruiz, Tomas; Martinez-Lozano, Carmen; Tomas, Virginia; Martin, Jesus

    2004-01-01

    A very sensitive fluorimetric method for the determination of menadione using a flow injection system is proposed. The method is based on the on-line reduction of menadione in dodecylsulphate micelles upon irradiation with UV light. The strong fluorescence of the reduced menadione in micellar medium is measured at 410 nm with excitation at 340 nm. The method shows a linear range between 2.42 and 245 ng ml -1 and a limit of detection of 0.18 ng ml -1 . The sample throughput was 90 injections per hour. The applicability of the assay was demonstrated by analysing this vitamin in commercial pharmaceutical preparations

  19. Flow injection gas chromatography with sulfur chemiluminescence detection for the analysis of total sulfur in complex hydrocarbon matrixes.

    Science.gov (United States)

    Hua, Yujuan; Hawryluk, Myron; Gras, Ronda; Shearer, Randall; Luong, Jim

    2018-01-01

    A fast and reliable analytical technique for the determination of total sulfur levels in complex hydrocarbon matrices is introduced. The method employed flow injection technique using a gas chromatograph as a sample introduction device and a gas phase dual-plasma sulfur chemiluminescence detector for sulfur quantification. Using the technique described, total sulfur measurement in challenging hydrocarbon matrices can be achieved in less than 10 s with sample-to-sample time ideal for fast analysis or trace sulfur analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Automation of radiochemical analysis by flow injection techniques. Am-Pu separation using TRU-resinTM sorbent extraction column

    International Nuclear Information System (INIS)

    Egorov, O.; Washington Univ., Seattle, WA; Grate, J.W.; Ruzicka, J.

    1998-01-01

    A rapid automated flow injection analysis (FIA) procedure was developed for efficient separation of Am and Pu from each other and from interfering matrix and radionuclide components using a TRU-resin TM column. Selective Pu elution is enabled via on-column reduction. The separation was developed using on-line radioactivity detection. After the separation had been developed, fraction collection was used to obtain the separated fractions. In this manner, a FIA instrument functions as an automated separation workstation capable of unattended operation. (author)

  1. Estimation of the quantification uncertainty from flow injection and liquid chromatography transient signals in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Laborda, Francisco; Medrano, Jesus; Castillo, Juan R.

    2004-01-01

    The quality of the quantitative results obtained from transient signals in high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) and flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) was investigated under multielement conditions. Quantification methods were based on multiple-point calibration by simple and weighted linear regression, and double-point calibration (measurement of the baseline and one standard). An uncertainty model, which includes the main sources of uncertainty from FI-ICPMS and HPLC-ICPMS (signal measurement, sample flow rate and injection volume), was developed to estimate peak area uncertainties and statistical weights used in weighted linear regression. The behaviour of the ICPMS instrument was characterized in order to be considered in the model, concluding that the instrument works as a concentration detector when it is used to monitorize transient signals from flow injection or chromatographic separations. Proper quantification by the three calibration methods was achieved when compared to reference materials, although the double-point calibration allowed to obtain results of the same quality as the multiple-point calibration, shortening the calibration time. Relative expanded uncertainties ranged from 10-20% for concentrations around the LOQ to 5% for concentrations higher than 100 times the LOQ

  2. Dual-phase gas-permeation flow-injection thermometric analysis for the determination of carbon dioxide.

    Science.gov (United States)

    Liu, S J; Tubino, M

    1998-11-01

    A flow-injection configuration based on a dual-phase gas-permeation system from a liquid donor to a gas acceptor stream with a thermistor flow-through detector is proposed for the direct analysis of the gas in the acceptor. This system was applied for the determination of carbon dioxide (in the form of carbonate) using the following chemical reaction: CO(2)(g)+2NH(3)(g)+H(2)O(g)=(NH(4))(2)CO(3)(s), with a linear response from 1x10(-3) to 50x10(-3) mol l(-1) of CO(3)(2-). Carbon dioxide was produced in the liquid donor and permeated into the gaseous acceptor stream of air/water vapor. The detection limit is 1x10(-3) mol l(-1) of carbonate, and a sampling frequency of 60 h(-1) is achieved with a relative standard deviation of 4.1% for replicate injections. The dual-phase gas-permeation flow-injection manifold, along with the membrane and phase separations, as well as the chemical reaction, provides enhanced selectivity when compared with the system employing a liquid acceptor stream, as serious interferents in this system, for instance, acetate and formate, among others, do not interfere in the proposed system.

  3. Chemiluminescent determination of vanadium(IV) using a cinchomeronic hydrazide-H2O2 system and flow injection analysis

    International Nuclear Information System (INIS)

    Pradana Perez, J.A.; Alegria, J.S. Durand; Hernando, P. Fernandez; Sierra, A. Narros

    2005-01-01

    This paper proposes a new chemiluminescent flow injection analysis (FIA) method for the determination of vanadium(IV) ions in aqueous media. The method is based on the chemiluminescent reaction that occurs between cinchomeronic hydrazide (CH) and hydrogen peroxide in a strongly alkaline medium, in which vanadium(IV) acts as a catalyst. The chemical and physical variables involved in the flow injection system are optimised using a modified simplex method. Vanadium ions can be detected in the 0.08 and 1.00 μg mL -1 range; the detection limit for a signal-to-noise ratio of 3 is 0.08 μg mL -1 . Great variations in the quantum yield were observed when cobalt(II), chromium(III), copper(II) and/or nickel(II) were present in the reaction medium. The proposed method is selective and simple, and can be successfully used to analyse water samples without the need for separation or preconcentration processes

  4. Determination of tellurium in lead and lead alloy using flow injection-hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Mesko, Marcia F.; Pozebon, Dirce; Flores, Erico M.M.; Dressler, Valderi L.

    2004-01-01

    A method based on flow injection-hydride generation atomic absorption spectrometry (FI-HG AAS) for the determination of trace amount of Te in lead and lead alloy is described. A flow injection system (FI) and related analytical parameters as well as Te determination and interference caused by Pb, Bi and Ag on Te were investigated. The Pb interference could be overcome by using a small sample volume, while the Bi interference could be overcome by thiourea. However, it was not possible to minimise the interference caused by Ag on Te. The optimised conditions for Te determination in the analysed samples were: 6 mol l -1 HCl as sample carrier solution, 0.75% (m/v) sodium tetrahydroborate as Te reductant, 40 μl of sample solution, and 200 ml min -1 Ar flow rate as carrier gas. The limit of quantification (LOQ) was 1.0 μg g -1 Te (using 250 mg of sample in 50 ml final solution), the limit of detection (LOD) was 2.5 μg l -1 and the relative standard deviation (RSD) was 6% for five consecutive measurements of sample solution. The standard addition calibration method was used. Relatively high sample throughput (ca. 45 sample runs can be performed in a working hour), reduced sample manipulation since matrix separation is not necessary, and minor waste generation are the main advantages of the proposed method for Te determination by FI-HG AAS

  5. Amperometric sensor for carbon dioxide: design, characteristics, and perforance

    International Nuclear Information System (INIS)

    Evans, J.; Pletcher, D.; Warburton, P.R.G.; Gibbs, T.K.

    1989-01-01

    A new sensor for atmospheric carbon dioxide is described. It is an amperometric device based on a porous electrode in a three-electrode cell and the electrolyte is a copper diamine complex in aqueous potassium chloride. The platinum cathode, held at constant potential, is used to detect the formation of Cu 2+ following the change in the pH of the solution when the sensor is exposed to an atmosphere containing carbon dioxide. The sensor described is designed to monitor carbon dioxide concentrations in the range 0-5%, although with some modifications, other ranges would be possible. The response to a change in the carbon dioxide content of the atmosphere is rapid (about 10s) while the monitored current is strongly (but nonlinearly) dependent on carbon dioxide concentration. Unlike other amperometric devices for carbon dioxide, there is no interference from oxygen although other acid gases would lead to an interfering response

  6. Amperometric titration of indium with edta solution in propanol

    International Nuclear Information System (INIS)

    Gevorgyan, A.M.; Talipov, Sh.T.; Khadeev, V.A.; Kostylev, V.S.; Khadeeva, L.A.

    1980-01-01

    Optimum conditions have been chosen for titration of indium with EDTA solution in anhydrous propanol and its mixtures with some aprotic solvents using amperometric and point detection. A procedure is suggested of determining indium microcontents in the presence of large amounts of other elements. The procedure is based on its extraction preseparation followed by direct titration in the extract with a standard EDTA solution [ru

  7. Development of a Telemetric, Miniaturized Electrochemical Amperometric Analyzer

    OpenAIRE

    Jaehyo Jung; Jihoon Lee; Siho Shin; Youn Tae Kim

    2017-01-01

    In this research, we developed a portable, three-electrode electrochemical amperometric analyzer that can transmit data to a PC or a tablet via Bluetooth communication. We performed experiments using an indium tin oxide (ITO) glass electrode to confirm the performance and reliability of the analyzer. The proposed analyzer uses a current-to-voltage (I/V) converter to convert the current generated by the reduction-oxidation (redox) reaction of the buffer solution to a voltage signal. This signa...

  8. Interaction of molybdenum (6) with potassium benzyldithiocarbaminate during amperometric titration

    International Nuclear Information System (INIS)

    Galushko, S.V.; Usatenko, Yu.I.

    1975-01-01

    The paper is an amperometric study of the mechanism of interaction between molybdenum (VI) and potassium benzyl dithiocarbamate [BDTC] which was based on the use of voltamperometry, electron paramagnetic resonance, infrared spectroscopy, potentiometry and elemental analysis. In amperometric titration Mo(VI) with BDTC (pH 4-2) forms a red compound of low solubility. In more acidic media the intensity of coloration is increased and a violet hue develops. On the basis of the data obtained it is concluded that in the amperometric titration of Mo(VI) with potassium BDTC there is first formation of a Mo(VI) compound, which subsequently acquires a red colour as a result of the reduction of Mo(VI) to Mo(V). It was also established that the degree of reduction is small where titration is carried out in the range pH 4.8-0.1. Quantitative determination of Mo is performed most effectively in slightly acidic media. Mo reacts with potassium BDTC in a ratio of 1:2. (E.P.)

  9. The determination of levofloxacin by flow injection analysis using UV detection, potentiometry, and conductometry in pharmaceutical preparations.

    Science.gov (United States)

    Altiokka, G; Atkosar, Z; Can, N O

    2002-10-15

    A flow injection analysis (FIA) using UV detection, potentiometry and conductometry for levofloxacin (LVF) are described in this study. The best solvent system was found to consist of 0.2 M acetate buffer at pH 3 having 10% MeOH. A flow rate of 1 ml min(-1) was pumped and active material was detected at 288 nm. The detection limit (LOD) and limit of quantification (LOQ) for FIA were calculated to be 3 x 10(-7) M (S/N = 3) and 1 x 10(-7) M (S/N = 10), respectively. In the analysis of tablets, the RSD values were found to be 0.83, 0.98 and 0.99 for FIA, potentiometric and conductometric methods, respectively. Copyright 2002 Elsevier Science B.V.

  10. Start-up assist by magnetized plasma flow injection in TPE-RX reversed-field pinch

    Energy Technology Data Exchange (ETDEWEB)

    Asai, T. [College of Science and Technology, Nihon University, 1-8 Kanda-Surugadai, Chiyoda-ku, Tokyo 101-8308 (Japan)]. E-mail: asai@phys.cst.nihon-u.ac.jp; Nagata, M. [Graduate School of Engineering, University of Hyogo, Himeji (Japan); Koguchi, H. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan); Hirano, Y. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan); Sakakita, H. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan); Yambe, K. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan); Kiyama, S. [National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan)

    2006-11-15

    A reversed-field pinch (RFP) start-up assisted by a magnetized plasma flow injection was demonstrated for the first time on a TPE-RX machine. This sequence of experiments aimed to establish a new method of ionization, gas-fill and helicity injection in the start-up phase of an RFP. In this start-up method, magnetized and well-ionized plasma is formed by a magnetized coaxial plasma gun and injected into the torus chamber as an initial pre-ionized plasma for RFP formation. In the initial experiments, attenuated density pump-out and comparatively slow decay of the toroidal flux and plasma current were observed as evidence of its being an effective start-up method.

  11. Flow Injection Analysis of Mercury Using 4-(Dimethylamino Benzaldehyde-4-Ethylthiosemicarbazone as the Ionophore of a Coated Wire Electrode

    Directory of Open Access Journals (Sweden)

    Sulaiman Ab Ghani

    2012-11-01

    Full Text Available A flow injection analysis (FIA incorporating a thiosemicarbazone-based coated wire electrode (CWE was developed method for the determination of mercury(II. A 0.1 M KNO3 carrier stream with pH between 1 and 5 and flow rate of 1 mL·min−1 were used as optimum parameters. A linear plot within the concentration range of 5 × 10−6–0.1 M Hg(II, slope of 27.8 ± 1 mV per decade and correlation coefficient (R2 of 0.984 were obtained. The system was successfully applied for the determination of mercury(II in dental amalgam solutions and spiked environmental water samples. Highly reproducible measurements with relative standard deviation (RSD < 1% (n = 3 were obtained, giving a typical throughput of 30 samples·h−1.

  12. Flow Injection/Sequential Injection Analysis Systems: Potential Use as Tools for Rapid Liver Diseases Biomarker Study

    Directory of Open Access Journals (Sweden)

    Supaporn Kradtap Hartwell

    2012-01-01

    Full Text Available Flow injection/sequential injection analysis (FIA/SIA systems are suitable for carrying out automatic wet chemical/biochemical reactions with reduced volume and time consumption. Various parts of the system such as pump, valve, and reactor may be built or adapted from available materials. Therefore the systems can be at lower cost as compared to other instrumentation-based analysis systems. Their applications for determination of biomarkers for liver diseases have been demonstrated in various formats of operation but only a few and limited types of biomarkers have been used as model analytes. This paper summarizes these applications for different types of reactions as a guide for using flow-based systems in more biomarker and/or multibiomarker studies.

  13. A novel flow injection chemiluminescence method for automated and miniaturized determination of phenols in smoked food samples.

    Science.gov (United States)

    Vakh, Christina; Evdokimova, Ekaterina; Pochivalov, Aleksei; Moskvin, Leonid; Bulatov, Andrey

    2017-12-15

    An easily performed fully automated and miniaturized flow injection chemiluminescence (CL) method for determination of phenols in smoked food samples has been proposed. This method includes the ultrasound assisted solid-liquid extraction coupled with gas-diffusion separation of phenols from smoked food sample and analytes absorption into a NaOH solution in a specially designed gas-diffusion cell. The flow system was designed to focus on automation and miniaturization with minimal sample and reagent consumption by inexpensive instrumentation. The luminol - N-bromosuccinimide system in an alkaline medium was used for the CL determination of phenols. The limit of detection of the proposed procedure was 3·10 -8 ·molL -1 (0.01mgkg -1 ) in terms of phenol. The presented method demonstrated to be a good tool for easy, rapid and cost-effective point-of-need screening phenols in smoked food samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. A novel approach for determination of free fatty acids in vegetable oils by a flow injection system with manual injection.

    Science.gov (United States)

    Ayyildiz, H Filiz; Kara, Huseyin; Sherazi, S T H

    2011-12-01

    A non-aqueous flow injection method for determining free fatty acid (FFA) content in corn and sunflower oil samples was developed. A single-line manifold system was built by modification of an HPLC for flow injection analysis (FIA). Without pre-treatment, oil samples were injected into a n-propanol solution containing KOH and phenolphthalein (PHP). The main parameters, such as flow rate of carrier phase, length, geometry, inner diameters of the coils and reagent concentration were all optimized. The proposed FIA method was validated for precision, accuracy, linear region, limit of detection (LOD) and limit of quantification (LOQ). The intra- and inter-day measurements of the precision of the method were found to be within the limits of acceptance criteria (RSD analyst. The linear concentration range was calculated as 0.09-1.50 and 0.07-1.40 FFA% for corn and sunflower oils, correspondingly. The LOD and LOQ were found to be 7.53 × 10(-4)-2.28 × 10(-3) oleic acid % and 7.11 × 10(-4)-2.23 × 10(-3) oleic acid % for corn and sunflower oils, respectively. The results were compared with those obtained by the AOCS (Ca-5a-40) method using statistical t and F tests, and a significant difference was not observed between the methods at a 95% confidence level. The proposed method is suitable for quality control of routine applications due to its simplicity, high sample throughput, and economy of solvents and sample, offering considerable promise as a low cost analytical system that needs minimum human intervention over long periods of time.

  15. Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

    Energy Technology Data Exchange (ETDEWEB)

    Shahida, Shabnam; Khan, Muhammad Haleem [Univ. of Azad Jammu and Kashmir, Muzaffarabad (Pakistan). Dept. of Chemistry; Ali, Akbar [Pakistan Institute of Nuclear Science and Technology, Islamabad (Pakistan). Chemistry Div.

    2014-02-15

    A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L{sup -1} levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min{sup -1}. The trapped complex was then eluted with 3.6 mol L{sup -1} HCl at a flow rate of 4.9 mL min{sup -1}. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L{sup -1} HCl stabilized with 1 % triton X-100, 4.9 mL min{sup -1}) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h{sup -1}, the enhancement factor was 97, the detection limit was 0.25 μg L{sup -1}, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L{sup -1}), whereas for 300 s of the preconcentration time and a sample frequency of 10 h{sup -1}, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L{sup -1} and the precision of 1.32 % (at 10 μg L{sup -1}) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

  16. Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

    International Nuclear Information System (INIS)

    Shahida, Shabnam; Khan, Muhammad Haleem; Ali, Akbar

    2014-01-01

    A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L"-"1 levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min"-"1. The trapped complex was then eluted with 3.6 mol L"-"1 HCl at a flow rate of 4.9 mL min"-"1. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L"-"1 HCl stabilized with 1 % triton X-100, 4.9 mL min"-"1) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h"-"1, the enhancement factor was 97, the detection limit was 0.25 μg L"-"1, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L"-"1), whereas for 300 s of the preconcentration time and a sample frequency of 10 h"-"1, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L"-"1 and the precision of 1.32 % (at 10 μg L"-"1) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

  17. Second-order Data by Flow Injection Analysis with Spectrophotometric Diode-array Detection and Incorporated Gel-filtration Chromatographic Column

    DEFF Research Database (Denmark)

    Bechmann, Iben Ellegaard

    1997-01-01

    A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate(III) and he......A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate...

  18. Amperometric biosensor for total monoamines using a glassy carbon paste electrode modified with human monoamine oxidase B and manganese dioxide particles

    International Nuclear Information System (INIS)

    Aigner, Maximilian; Telsnig, Dietlind; Teubl, Christian; Ortner, Astrid; Kalcher, Kurt; Macheroux, Peter; Wallner, Silvia; Edmondson, Dale

    2015-01-01

    We have prepared a biosensor for the determination of the total monoamine content in complex matrices by immobilizing a human monoamine oxidase B (hMAO B) on a glassy carbon paste electrode and adding manganese dioxide microparticles as the mediator. The enzyme hMAO B (expressed in Pichia pastoris and immobilized by using a dialysis membrane) catalyzes the oxidative deamination of monoamines, and this results in the formation of the corresponding aldehyde, ammonia and hydrogen peroxide. The latter was detected at pH 7.5 at a working voltage of 400 mV (vs. Ag/AgCl) by differential pulse voltammetry and amperometrically by applying flow injection analysis. Analytical parameters were established by using phenylethylamine (PEA) as a standard substrate. Peak height and concentration of PEA are linearly related in the 0.5 to 150 μg mL −1 concentration range, and the limits of detection and of quantification are 0.15 and 0.5 μg mL −1 of PEA, respectively. Substrate specificity was investigated with different monoamines including PEA, serotonin, benzylamine, dopamine, tyramine, and norepinephrine. The applicability of the biosensor was successfully tested in a commercial fish sauce that served as a complex matrix. The total monoamine content was calculated as PEA-equivalents. (author)

  19. Flow injection on-line dilution for multi-element determination in human urine with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Gammelgaard, Bente

    2001-01-01

    A simple flow injection on-line dilution procedure with detection by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of copper, zinc, arsenic, lead, selenium, nickel and molybdenum in human urine. Matrix effects were minimized by employing a dilution factor...

  20. Rapid isolation of biomarkers for compound specific radiocarbon dating using high-performance liquid chromatography and flow injection analysis-atmospheric pressure chemical ionisation mass spectrometry

    NARCIS (Netherlands)

    Sinninghe Damsté, J.S.; Smittenberg, R.H.; Hopmans, E.C.; Schouten, S.

    2002-01-01

    Repeated semi-preparative normal-phase HPLC was performed to isolate selected biomarkers from sediment extracts for radiocarbon analysis. Flow injection analysis mass spectrometry was used for rapid analysis of collected fractions to evaluate the separation procedure, taking only 1 min per fraction.

  1. On-line Speciation of Cr(III) and Cr(VI) by Flow Injection Analysis With Spectrophotometric Detection and Chemometrics

    DEFF Research Database (Denmark)

    Diacu, Elena; Andersen, Jens Enevold Thaulov

    2003-01-01

    A flow injection system has been developed, for on-line speciation. of Cr(III) and Cr(VI) by the Diphenylcarbazide (DPC) method with H2O2 oxidation followed by spectrophotometric detection at the 550 nm wavelength. The data thus obtained were subjected to a chemometric analysis (PLS), which showe...

  2. Investigations into the Role of Modifiers for Entrapment of Hydrides in Flow Injection Hydride Generation Electrothermal Atomic Absorption Spectrometry as Exemplified for the Determination of Germanium

    DEFF Research Database (Denmark)

    Hilligsøe, Bo; Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

    1997-01-01

    Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is...

  3. Rapid determination of 99Tc in environmental samples by high resolution ICP-MS coupled with on-line flow injection system

    International Nuclear Information System (INIS)

    Kim, C.K.; Kim, C.S.; Rho, B.H.; Lee, J.I.

    2002-01-01

    High resolution inductively coupled plasma mass spectrometry coupled with an on-line flow injection system (FI-HR-ICP-MS) was applied to determine the ultra-trace level 99 Tc in soil. The flow injection system (PrepLab TM ) was composed of two TEVA-Spec R resins, reduced remarkably the sample amounts and the analysis time, compared to the conventional analytical methods. In the flow injection system, Mo and Ru were sufficiently eliminated by using the flow injection system, with the decontamination factors of 1.6 x 10 4 and 9.9 x 10 5 , respectively. With the present method, it was possible to determine ultra-low level of 99 Tc in 3∼6 soil at 3-5 hours of analysis time per sample. The relative standard deviation for each sample was less than 4%. The detection limits for 99 Tc was 85 fg x ml -1 (0.05 mBq x ml -1 ), which was calculated from the three times standard deviation of the count rate of the blank. (author)

  4. Exploiting flow injection and sequential injection for trace metal determinations in conjunction with detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    and selectivity. Either in order to separate/preconcentrate the analyte material, or because of the presence of potentially interfering matrix constituents. Such pretreatments are advantageously performed in flow injection (FI) or sequential injection (SI) manifolds, where all appropriate unit operations can...

  5. Down scaled Kjeldahl digestion and flow injection conductometric system for determination of protein content in some traditional northern Thai foods.

    Science.gov (United States)

    Yanu, Pattama; Jakmunee, Jaroon

    2017-09-01

    A flow injection conductometric (FIC) system for determination of total Kjeldahl nitrogen (TKN) was developed for estimating total protein content in food. A small scale Kjeldahl digestion was performed with a short digestion time of only 20min. The digested solution was injected into the FIC system, and TKN was converted to ammonia gas in an alkaline donor stream of the system. The gas diffused through a membrane and dissolved into an acceptor stream causing an increase in conductivity as detected by a detector and recorded as a peak. Under the optimum condition, a linear calibration graph in the range of 4.00-100.00mgL -1 was obtained with LOD of 0.05mgL -1 . A good precision (0.04% RSD, n=11, 30.00mgNL -1 ) and high sample throughput of 72h -1 was achieved. The method was applied for determination of protein in some traditional northern Thai foods, revealing that they are good sources of proteins. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Reverse flow injection spectrophotometric determination of ciprofloxacin in pharmaceuticals using iron from soil as a green reagent

    Science.gov (United States)

    Palamy, Sysay; Ruengsitagoon, Wirat

    2018-02-01

    A novel reverse flow injection spectrophotometric method for the determination of ciprofloxacin was successfully combined with the on-line introduction of an iron solution extracted from soil as green reagent. The assay was optimized by a univariate method to select the optimum conditions for the highest absorbance and highest stability of the complex. Beer-Lambert's law (λmax = 440 nm) is obeyed in the range 0.5-50 μg mL- 1 with a correlation coefficient (r2) of 0.9976 and 0.9996 using soil as green reagent from Khon Kaen, Thailand and Vientiane, Laos, respectively. The average percentage recoveries were in the range of 98.55-102.14% and the precision was in the range of 0.80-1.73%. The limit of detection and the limit of quantitation were 0.20 and 0.69 μg mL- 1, respectively, with a sampling rate of over 46 samples h- 1. The method was successfully applied to the determination of ciprofloxacin in commercial pharmaceutical formulations. The results were in good agreement with those obtained by the reference HPLC method using a t-test at 95% of confidence level for comparison. This method is suitable for laboratories looking for alternative analytical methods using green reagents.

  7. FLOW INJECTION ANALYSIS SYSTEM COUPLED WITH ICP-EOS FOR DETERMINATION OF SOME METALLIC ELEMENTS IN DRINKING WATER

    Directory of Open Access Journals (Sweden)

    Cristina Dinu

    2009-06-01

    Full Text Available The European Drinking Water Directive (98/83/EC, transposed in Romanian Legislation as Low 458/2002, amended by Low 311/2004, imposes the limit of concentration for metallic elements in water intended for human consumption. The toxic metals arsenic and selenium are among these elements and the limit value is 10 μg/L. In the paper there are presented the working conditions for determination of As and Se from drinking water using modern techniques based on the fl ow injection-hydride generation with the inductively coupled plasma atomic emission spectrometry (FIAS-ICP-EOS. The analyses were performed on Optima 5300 DV Perkin Elmer equipment with FIAS 400 Flow Injection System, Perkin Elmer type. For the hydride generation two types of solution were used: 10% (v/v HCl as a carrier solution and 0.2 % NaBH4 in 0.05%NaOH solution as a reducing agent [1]. The treatment step of the samples and standard solutions consisted in reducing with mixed solutions of KI and ascorbic acid in acidic condition (HCl for As and only with HCl and high temperature for Se [2,3]. The paper contains the characteristic parameters of the methods, such as: low detection limit, quantifi cation limit, repeatability, precision, recovery, which were evaluated using Certifi ed Reference Materials for each element.

  8. An automatic flow injection analysis procedure for photometric determination of ethanol in red wine without using a chromogenic reagent.

    Science.gov (United States)

    Borges, Sivanildo S; Frizzarin, Rejane M; Reis, Boaventura F

    2006-05-01

    An automatic reagentless photometric procedure for the determination of ethanol in red wine is described. The procedure was based on a falling drop system that was implemented by employing a flow injection analysis manifold. The detection system comprised an infrared LED and a phototransistor. The experimental arrangement was designed to ensure that the wine drop grew between these devices, thus causing a decrease in the intensity of the radiation beam coming from the LED. Since ethanol content affected the size of the wine drop this feature was exploited to develop an analytical procedure for the photometric determination of ethanol in red wine without using a chromogenic reagent. In an attempt to prove the usefulness of the proposed procedure, a set of red wines were analysed. No significant difference between our results and those obtained with a reference method was observed at the 95% confidence level. Other advantages of our method were a linear response ranging from 0.17 up to 5.14 mol L(-1) (1.0 up to 30.0%) ethanol (R = 0.999); a limit of detection of 0.05 mol L(-1) (0.3%) ethanol; a relative standard deviation of 2.5% (n = 10) using typical wine sample containing 2.14 mol L(-1) (12.5%) ethanol; and a sampling rate of 50 determinations per hour.

  9. Flow Injection Analysis with Electrochemical Detection for Rapid Identification of Platinum-Based Cytostatics and Platinum Chlorides in Water

    Directory of Open Access Journals (Sweden)

    Marketa Kominkova

    2014-02-01

    Full Text Available Platinum-based cytostatics, such as cisplatin, carboplatin or oxaliplatin are widely used agents in the treatment of various types of tumors. Large amounts of these drugs are excreted through the urine of patients into wastewaters in unmetabolised forms. This phenomenon leads to increased amounts of platinum ions in the water environment. The impacts of these pollutants on the water ecosystem are not sufficiently investigated as well as their content in water sources. In order to facilitate the detection of various types of platinum, we have developed a new, rapid, screening flow injection analysis method with electrochemical detection (FIA-ED. Our method, based on monitoring of the changes in electrochemical behavior of analytes, maintained by various pH buffers (Britton-Robinson and phosphate buffer and potential changes (1,000, 1,100 and 1,200 mV offers rapid and cheap selective determination of platinum-based cytostatics and platinum chlorides, which can also be present as contaminants in water environments.

  10. A Customizable Flow Injection System for Automated, High Throughput, and Time Sensitive Ion Mobility Spectrometry and Mass Spectrometry Measurements.

    Science.gov (United States)

    Orton, Daniel J; Tfaily, Malak M; Moore, Ronald J; LaMarche, Brian L; Zheng, Xueyun; Fillmore, Thomas L; Chu, Rosalie K; Weitz, Karl K; Monroe, Matthew E; Kelly, Ryan T; Smith, Richard D; Baker, Erin S

    2018-01-02

    To better understand disease conditions and environmental perturbations, multiomic studies combining proteomic, lipidomic, and metabolomic analyses are vastly increasing in popularity. In a multiomic study, a single sample is typically extracted in multiple ways, and various analyses are performed using different instruments, most often based upon mass spectrometry (MS). Thus, one sample becomes many measurements, making high throughput and reproducible evaluations a necessity. One way to address the numerous samples and varying instrumental conditions is to utilize a flow injection analysis (FIA) system for rapid sample injections. While some FIA systems have been created to address these challenges, many have limitations such as costly consumables, low pressure capabilities, limited pressure monitoring, and fixed flow rates. To address these limitations, we created an automated, customizable FIA system capable of operating at a range of flow rates (∼50 nL/min to 500 μL/min) to accommodate both low- and high-flow MS ionization sources. This system also functions at varying analytical throughputs from 24 to 1200 samples per day to enable different MS analysis approaches. Applications ranging from native protein analyses to molecular library construction were performed using the FIA system, and results showed a highly robust and reproducible platform capable of providing consistent performance over many days without carryover, as long as washing buffers specific to each molecular analysis were utilized.

  11. Flow injection chemiluminescent determination of N-nitrosodimethylamine using photogenerated tris(2,2'-bipyridyl) ruthenium (III)

    International Nuclear Information System (INIS)

    Perez-Ruiz, Tomas; Martinez-Lozano, Carmen; Tomas, Virginia; Martin, Jesus

    2005-01-01

    A flow injection configuration was developed and evaluated for the chemiluminescent determination of N-nitrosodimethylamine. The method is based on the on-line cleavage of the N-NO bond of the nitrosamine by irradiation with ultraviolet light. The dimethylamine generated was subsequently reacted with tris(2,2'-bipyridyl) ruthenium (III), which was generated through the on-line photo-oxidation of tris(2,2'-bipyridyl) ruthenium (II) with peroxydisulfate. After selecting the best operating parameters, the emitted light showed a linear relationship with the concentration of N-nitrosodimethylamine between 1.5 and 148 ng ml -1 , with a detection limit of 0.29 ng ml -1 . The repeatability was 1.6% expressed as relative standard deviation (n = 10) and the reproducibility, studied on five consecutive days, was 3.2%. The sample throughput was 50 injections per hour. The method was applied to studying the recoveries of N-nitrosodimethylamine in water and different cured meat products

  12. Flow-Injection Solid Phase Partial Least-Squares Spectrophotometric Simultaneous Determination of Iron, Nickel and Zinc

    Directory of Open Access Journals (Sweden)

    Teixeira Leonardo S. G.

    2002-01-01

    Full Text Available A PLS-2 multivariate calibration method has been developed for the simultaneous determination of iron, nickel and zinc in ternary mixtures by solid phase spectrophotometry associated with flow injection analysis. Fe(II, Ni(II and Zn(II form color complexes with 1-(2-thiazolylazo-2-naphthol (TAN, immobilized on a C18 bonded silica support, at pH 6.4. The proposed procedure is based on the different reaction/retention ratios of the studied ions on the solid support. Bilinear spectrophotometric data of the analytes, fixed in the solid support, were recorded in the 400-800 nm wavelength range as a function of time and a partial least squares (PLS-2 algorithm was used to predict results of synthetic samples. The calibration set employed was integrated by 8 ternary mixture standards and a blank solution. Mixtures containing 0.040 to 0.20 mg L-1, of each species, were successfully resolved, using 3 factors for each analyte and a restricted number of absorbance data obtained in the wavelength range from 560 to 650 nm.

  13. New method for simultaneous determination of Fe(II) and Fe(III) in water using flow injection technique

    International Nuclear Information System (INIS)

    Kozak, J.; Gutowski, J.; Kozak, M.; Wieczorek, M.; Koscielniak, P.

    2010-01-01

    The method exploits the possibilities of flow injection gradient titration in a system of reversed flow with spectrophotometric detection. In the developed approach a small amount of titrant (EDTA) is injected into a stream of sample containing a mixture of indicators (sulfosalicylic acid and 1,10-phenanthroline). In acid environment sulfosalicylic acid forms a complex with Fe(III), whereas 1,10-phenanthroline forms a complex with Fe(II). Measurements are performed at wavelength λ = 530 nm when radiation is absorbed by both complexes. After injection EDTA replaces sulfosalicylic acid and forms with Fe(III) more stable colourless complex. As a result, a characteristic 'cut off' peak is registered with a width corresponding to the Fe(III) concentration and with a height corresponding to the Fe(II) concentration. Calibration was performed by titration of four two-component standard solutions of the Fe(II)/Fe(III) concentrations established in accordance with 2 2 factorial plan. The method was tested with the use of synthetic samples and then it was applied to the analysis of water samples taken from artesian wells. Under optimized experimental conditions Fe(II) and Fe(III) were determined with precision less than 0.8 and 2.5% (RSD) and accuracy less than 3.2 and 5.1% (relative error) within the concentration ranges of 0.1-3.0 and 0.9-3.5 mg L -1 of both analytes, respectively.

  14. Sequential determination of multi-nutrient elements in natural water samples with a reverse flow injection system.

    Science.gov (United States)

    Lin, Kunning; Ma, Jian; Yuan, Dongxing; Feng, Sichao; Su, Haitao; Huang, Yongming; Shangguan, Qipei

    2017-05-15

    An integrated system was developed for automatic and sequential determination of NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ in natural waters based on reverse flow injection analysis combined with spectrophotometric detection. The system operation was controlled by a single chip microcomputer and laboratory-programmed software written in LabVIEW. The experimental parameters for each nutrient element analysis were optimized based on a univariate experimental design, and interferences from common ions were evaluated. The upper limits of the linear range (along with detection limit, µmolL -1 ) of the proposed method was 20 (0.03), 200 (0.7), 12 (0.3), 5 (0.03), 5 (0.03), 9 (0.2) µmolL -1 , for NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ , respectively. The relative standard deviations were below 5% (n=9-13) and the recoveries varied from 88.0±1.0% to 104.5±1.0% for spiked water samples. The sample throughput was about 20h -1 . This system has been successfully applied for the determination of multi-nutrient elements in different kinds of water samples and showed good agreement with reference methods (slope 1.0260±0.0043, R 2 =0.9991, n=50). Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Detection of Total Phenol in Green and Black Teas by Flow Injection System and Unmodified Screen Printed Electrode

    Directory of Open Access Journals (Sweden)

    Ivanildo Luiz de Mattos

    2010-01-01

    Full Text Available A flow injection system using an unmodified gold screen-printed electrode was employed for total phenol determination in black and green teas. In order to avoid passivation of the electrode surface due to the redox reaction, preoxidation of the sample was realized by hexacyanoferrate(III followed by addition of an EDTA solution. The complex formed in the presence of EDTA minimizes or avoids polymerization of the oxidized phenols. The previously filtered tea sample and hexacyanoferrate(III reagent were introduced simultaneously into two-carrier streams producing two reproducible zones. At confluence point, the pre-oxidation of the phenolic compounds occurs while this zone flows through the coiled reactor and receives the EDTA solution before phenol detection. The consumption of ferricyanide was monitorized at 360 mV versus Ag/AgCl and reflected the total amount of phenolic compounds present in the sample. Results were reported as gallic acid equivalents (GAEs. The proposed system is robust, versatile, environmentally-friendly (since the reactive is used only in the presence of the sample, and allows the analysis of about 35–40 samples per hour with detection limit = 1 mg/L without the necessity for surface cleaning after each measurement. Precise results are in agreement with those obtained by the Folin-Ciocalteu method.

  16. Flow injection determination of hydrogen peroxide using catalytic effect of cobalt(II) ion on a dye formation reaction.

    Science.gov (United States)

    Kurihara, Makoto; Muramatsu, Miyuki; Yamada, Mari; Kitamura, Naoya

    2012-07-15

    A novel flow injection photometric method was developed for the determination of hydrogen peroxide in rainwater. This method is based on a cobalt(II)-catalyzed oxidative coupling of 3-methyl-2-benzothiazolinone hydrazone (MBTH) with N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3,5-dimethoxyaniline (DAOS) as a modified Trinder's reagent to produce intensely colored dye (λ(max)=530nm) in the presence of hydrogen peroxide at pH 8.4. In this method, 1,2-dihydroxy-3,5-benzenedisulfonic acid (Tiron) acted as an activator for the cobalt(II)-catalyzed reaction and effectively increased the peak height for hydrogen peroxide. The linear calibration graphs were obtained in the hydrogen peroxide concentration range 5×10(-8) to 2.2×10(-6)mol dm(-3) at a sampling rate of 20h(-1). The relative standard deviations for ten determinations of 2.2×10(-6) and 2×10(-7)mol dm(-3) hydrogen peroxide were 1.1% and 3.7%, respectively. The proposed method was successfully applied to the determination of hydrogen peroxide in rainwater samples and the analytical results agreed fairly well with the results obtained by different two reference methods; peroxidase method and hydrogen peroxide electrode method. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Determination of hydrogen peroxide in water by chemiluminescence detection, (1). Flow injection type hydrogen peroxide detection system

    International Nuclear Information System (INIS)

    Yamashiro, Naoya; Uchida, Shunsuke; Satoh, Yoshiyuki; Morishima, Yusuke; Yokoyama, Hiroaki; Satoh, Tomonori; Sugama, Junichi; Yamada, Rie

    2004-01-01

    A flow injection type hydrogen peroxide detection system with a sub-ppb detection limit has been developed to determine hydrogen peroxide concentration in water sampled from a high temperature, high pressure hydrogen peroxide water loop. The hydrogen peroxide detector is based on luminol chemiluminescence spectroscopy. A small amount of sample water (20 μl) is mixed with a reagent mixture, an aqueous solution of luminol and Co 2+ catalyst, in a mixing cell which is installed just upstream from the detection cell. The optimum values for pH and the concentrations of luminol and Co 2+ ion have been determined to ensure a lower detectable limit and a higher reproducibility. The photocurrent detected by the detection system is expressed by a linear function of the hydrogen peroxide concentration in the region of lower concentration ([H 2 O 2 ] 2 O 2 ] in the region of higher concentration ([H 2 O 2 ] > 10 ppb). The luminous intensity of luminol chemiluminescence is the highest when pH of the reagent mixture is 11.0. Optimization of the major parameters gives the lowest detectable limit of 0.3 ppb. (author)

  18. Carbon paste electrode modified with silver thimerosal for the potentiometric flow injection analysis of silver(I)

    Energy Technology Data Exchange (ETDEWEB)

    Ibrahim, Hosny [Chemistry Department, Faculty of Science, Cairo University, Cairo (Egypt)]. E-mail: dr_hosny@yahoo.com

    2005-07-27

    The utility of carbon paste electrode modified with silver ethylmercurythiosalicylate (silver thimerosal) in both static mode and flow injection analysis (FIA) is demonstrated. The electrode was fully characterized in terms of composition, response time, thermal stability, usable pH and ionic strength ranges. It has been shown that diisononyl phthalate (DINP) acts as more suitable solvent mediator for preparation of the electrode, which exhibits linear response range to Ag(I) extending from 5.0 x 10{sup -7} to 1.0 x 10{sup -3} M with detection limit of 2.5 x 10{sup -7} M and Nernstian slope of 59.3 {+-} 1.0 mV/decade. The proposed chemically modified carbon paste electrode shows a very good selectivity for Ag(I) over a wide variety of metal ions and successfully used for the determination of the silver content of silver sulphadiazine (burning cream) and developed radiological films. The electrode was also used as an indicator electrode in the potentiometric titration of thiopental and thimerosal with AgNO{sub 3}.

  19. Spectrophotometric flow-injection determination of sulphite in white wines involving gas diffusion through a concentric tubular membrane

    Directory of Open Access Journals (Sweden)

    Melo Denise

    2003-01-01

    Full Text Available A flow-injection system is proposed for the spectrophotometric determination of sulphite in white wines. The method involves analyte conversion to SO2, gas diffusion through a Teflon® semi-permeable membrane, collection into an alkaline stream (pH 8, reaction with Malachite green (MG and monitoring at 620 nm. With a concentric tubular membrane, the system design was simplified. Influence of reagent concentrations, pH of donor and acceptor streams, temperature, timing, surfactant addition and presence of potential interfering species of the wine matrix were investigated. A pronounced (ca. 100% enhancement in sensitivity was noted by adding cetylpyridinium chloride (CPC. The proposed system is robust and baseline drift is not observed during 4 h operating periods. Only 400 muL of sample and 0.32 mg MG are required per determination. The system handles 30 samples per hour, yielding precise results (r.s.d. < 0.015 for 1.0 - 20.0 mg L-1 SO2 in agreement with those obtained by an alternative procedure.

  20. Determination of thiram in natural waters using flow-injection with cerium(IV)-quinine chemiluminescence system.

    Science.gov (United States)

    Waseem, Amir; Yaqoob, Mohammad; Nabi, Abdul

    2010-01-01

    A simple and rapid flow-injection chemiluminescence method has been developed for the determination of dithiocarbamate fungicide thiram based on the chemiluminescence reaction of thiram with ceric sulfate and quinine in aqueous sulfuric acid. The present method allowed the determination of thiram in the concentration range of 7.5-2500 ng/mL and the detection limit (signal-to-noise ratio = 3) was 7.5 ng/mL with sample throughput of 120/h. The relative standard deviation was 2.5% for 10 replicate analyses of 500 ng/mL thiram. The effects of foreign species including various anions and cations present in water at environmentally relevant concentrations and some pesticides were also investigated. The proposed method was applied to determine thiram in spiked natural waters using octadecyl bonded phase silica (C(18)) cartridges for solid-phase extraction. The recoveries were in the range 99 +/- 1 to 104 +/- 1%. Copyright (c) 2009 John Wiley & Sons, Ltd.

  1. Flow Injection Photosensitized Chemiluminescence of Luminol with Cu(II-Rose Bengal: Mechanistic Approach and Vitamin A and C Determination

    Directory of Open Access Journals (Sweden)

    Muhammad Asgher

    2014-01-01

    Full Text Available Rose Bengal photosensitized flow injection chemiluminescence method is reported using luminol-Cu(II for the determination of vitamins A and C in pharmaceutical formulations. The reaction is based on the enhancement effect of analyte in the production of anion radicals of Rose Bengal (RB•− which rapidly interact with dissolved oxygen and generate superoxide anions radicals (O2•− and hydrogen peroxide (H2O2. Highly reactive hydroxyl radicals (•OH were produced via dismutation of H2O2 by catalyst (Cu2+. The generated superoxide anions radicals and hydroxyl radicals thus oxidize luminol in alkaline medium to generate strong chemiluminescence. The limit of detection (3s of the blank, n=6 of vitamins A and C and RB was found to be 0.008, 0.005, and 0.05 μg mL−1, respectively. The sample throughput of 70 h−1 for vitamins A and C and 30 h−1 for RB was found. Calibration curve was linear in the range of 0.05–15, 0.01–20, and 0.1–50 μg mL−1 for vitamins A and C and RB, respectively, with relative standard deviations (RSDs; n=3 in the range 1.6–3.6%. The method was successfully applied to pharmaceutical formulations and the results obtained were in good agreement with the labeled values.

  2. Flow injection chemiluminescence determination of lercanidipine based on N-chlorosuccinimide-eosin Y post-chemiluminescence reaction.

    Science.gov (United States)

    Wang, Guowei; Zhao, Fang; Gao, Ying

    2014-12-01

    A novel post-chemiluminescence (PCL) reaction was discovered when lercanidipine was injected into the CL reaction mixture of N-chlorosuccinimide with alkaline eosin Y in the presence of cetyltrimethylammonium bromide (CTAB), where eosin Y was used as the CL reagent and CTAB as the surfactant. Based on this observation, a simple and highly sensitive PCL method combined with a flow injection (FI) technique was developed for the assay of lercanidipine. Under optimum conditions, the CL signal was linearly related to the concentration of lercanidipine in the range 7.0 × 10(-10) to 3.0 × 10(-6)  g/mL with a detection limit of 2.3 × 10(-10) g/mL (3σ). The relative standard deviation (RSD) was 2.1% for 1.0 × 10(-8) g/mL lercanidipine (n = 13). The proposed method had been applied to the estimation of lercanidipine in tablets and human serum samples with satisfactory results. The possible CL mechanism is also discussed briefly. Copyright © 2014 John Wiley & Sons, Ltd.

  3. A Customizable Flow Injection System for Automated, High Throughput, and Time Sensitive Ion Mobility Spectrometry and Mass Spectrometry Measurements

    Energy Technology Data Exchange (ETDEWEB)

    Orton, Daniel J. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Tfaily, Malak M. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Moore, Ronald J. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; LaMarche, Brian L. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Zheng, Xueyun [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Fillmore, Thomas L. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Chu, Rosalie K. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Weitz, Karl K. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Monroe, Matthew E. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Kelly, Ryan T. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Smith, Richard D. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States; Baker, Erin S. [Biological Sciences Division, Pacific Northwest National Laboratory, Richland, WA 99352, United States

    2017-12-13

    To better understand disease conditions and environmental perturbations, multi-omic studies (i.e. proteomic, lipidomic, metabolomic, etc. analyses) are vastly increasing in popularity. In a multi-omic study, a single sample is typically extracted in multiple ways and numerous analyses are performed using different instruments. Thus, one sample becomes many analyses, making high throughput and reproducible evaluations a necessity. One way to address the numerous samples and varying instrumental conditions is to utilize a flow injection analysis (FIA) system for rapid sample injection. While some FIA systems have been created to address these challenges, many have limitations such as high consumable costs, low pressure capabilities, limited pressure monitoring and fixed flow rates. To address these limitations, we created an automated, customizable FIA system capable of operating at diverse flow rates (~50 nL/min to 500 µL/min) to accommodate low- and high-flow instrument sources. This system can also operate at varying analytical throughputs from 24 to 1200 samples per day to enable different MS analysis approaches. Applications ranging from native protein analyses to molecular library construction were performed using the FIA system. The results from these studies showed a highly robust platform, providing consistent performance over many days without carryover as long as washing buffers specific to each molecular analysis were utilized.

  4. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS.

    Science.gov (United States)

    Bentlin, Fabrina R S; dos Santos, Clarissa M M; Flores, Erico M M; Pozebon, Dirce

    2012-01-13

    This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L(-1), respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Flow injection preconcentration system using a new functionalized resin for determination of cadmium and nickel in tobacco samples

    International Nuclear Information System (INIS)

    Lemos, Valfredo Azevedo; Novaes, Cleber Galvao; Lima, Adriana da Silva; Vieira, Daniel Rodrigues

    2008-01-01

    A solid-phase extraction method combined with flow injection (FI) on-line flame atomic absorption spectrometry (FAAS) for the determination of cadmium and nickel in tobacco samples is presented. The 2-aminothiophenol functionalized Amberlite XAD-4 (AT-XAD) resin was synthesized by covalent coupling of the ligand with the copolymer through a methylene group. A minicolumn packed with AT-XAD was connected into the automated on-line preconcentration system. Elution of metal ions from minicolumn can be made with 0.50 mol L -1 hydrochloric acid solution. With a consumption of 21.0 mL of sample solution, detection limits (3 s) of 0.3 (Cd) and 0.8 μg L -1 (Ni) were achieved at a sample throughput of 18 h -1 . Enrichment factors (EF) of 99 (cadmium) and 43 (nickel) were obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The contents of Cd and Ni in a certified reference material (NIST 1570a, spinach leaves) determined by the present method was in good agreement with the certified value. The developed procedure was also successfully applied to the determination of Cd and Ni in local tobacco samples

  6. Determination of trace elements in seawater by air-flow injection/ICP-MS with chelating resin preconcentration

    International Nuclear Information System (INIS)

    Lee, Kyue-Hyung; Ohshima, Mitsuko; Motomizu, Shoji

    2002-01-01

    Multielement determination of major to trace metals in a deep seawater malt was accomplished by inductively coupled plasma-mass spectrometry (ICP-MS) together with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Major elements, such as Na, K, Mg, and Ca, were measured by ICP-AES and normal continuos nebulization ICP-MS after sample dilution by 10 3 -10 6 fold. Fifteen trace elements in the concentrated metal solutions pretreated with cation-exchange resin or chelating resin could be simultaneously determined by air-flow injection/ICP-mass spectrometry (AFI/ICP-MS). Since the injection volume for AFI/ICP-MS was 25 μl, final samples volumes less than 500 μl were enough for several replicate measurements. Three different preconcentration methods assisted with AFI/ICP-MS were examined and could be successfully applied to a deep seawater malt. The analytical results of rate earth elements (REEs) and Co, Ni, Cu, Zn, Cd, and Pb obtained by AFI/ICP-MS coupled with disk filtration method using iminodiacetate (IDA)-type chelating resin were favorably agreed with the data obtained by AFI/ICP-MS coupled with column preconcentration method using chitosan-based chelating resin. (author)

  7. A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei, Behzad [Department of Chemistry, Isfahan University of Technology, Isfahan 84156-84111 (Iran, Islamic Republic of)], E-mail: rezaei@cc.iut.ac.ir; Keyvanfard, Mohsen [Faculty of Science, Majlesi Campus, Islamic Azad University, Isfahan (Iran, Islamic Republic of)

    2008-03-01

    In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at {lambda}{sub max} = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL ({delta}A = 0.2819C{sub Ru} + 1.1840) and 20.0-100.0 ng/mL ({delta}A = 0.0984C{sub Ru} + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 {+-} 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples.

  8. A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

    International Nuclear Information System (INIS)

    Rezaei, Behzad; Keyvanfard, Mohsen

    2008-01-01

    In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at λ max = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL (ΔA = 0.2819C Ru + 1.1840) and 20.0-100.0 ng/mL (ΔA = 0.0984C Ru + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 ± 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples

  9. Novel amperometric glucose biosensor based on MXene nanocomposite

    KAUST Repository

    Rakhi, R. B.

    2016-11-10

    A biosensor platform based on Au/MXene nanocomposite for sensitive enzymatic glucose detection is reported. The biosensor leverages the unique electrocatalytic properties and synergistic effects between Au nanoparticles and MXene sheets. An amperometric glucose biosensor is fabricated by the immobilization of glucose oxidase (GOx) enzyme on Nafion solubilized Au/ MXene nanocomposite over glassy carbon electrode (GCE). The biomediated Au nanoparticles play a significant role in facilitating the electron exchange between the electroactive center of GOx and the electrode. The GOx/Au/MXene/Nafion/GCE biosensor electrode displayed a linear amperometric response in the glucose concentration range from 0.1 to 18 mM with a relatively high sensitivity of 4.2 μAmM−1 cm−2 and a detection limit of 5.9 μM (S/N = 3). Furthermore, the biosensor exhibited excellent stability, reproducibility and repeatability. Therefore, the Au/MXene nanocomposite reported in this work is a potential candidate as an electrochemical transducer in electrochemical biosensors.

  10. Thick-film textile-based amperometric sensors and biosensors.

    Science.gov (United States)

    Yang, Yang-Li; Chuang, Min-Chieh; Lou, Shyh-Liang; Wang, Joseph

    2010-06-01

    The incorporation of amperometric sensors into clothing through direct screen-printing onto the textile substrate is described. Particular attention is given to electrochemical sensors printed directly on the elastic waist of underwear that offers tight direct contact with the skin. The textile-based printed carbon electrodes have a well-defined appearance with relatively smooth conductor edges and no apparent defects or cracks. Convenient voltammetric and chronoamperometric measurements of 0-3 mM ferrocyanide, 0-25 mM hydrogen peroxide, and 0-100 muM NADH have been documented. The favorable electrochemical behavior is maintained under folding or stretching stress, relevant to the deformation of clothing. The electrochemical performance and tolerance to mechanical stress are influenced by the physical characteristics of the textile substrate. The results indicate the potential of textile-based screen-printed amperometric sensors for future healthcare, sport or military applications. Such future applications would benefit from tailoring the ink composition and printing conditions to meet the specific requirements of the textile substrate.

  11. Novel amperometric glucose biosensor based on MXene nanocomposite

    KAUST Repository

    Baby, Rakhi Raghavan; Nayuk, Pranati; Xia, Chuan; Alshareef, Husam N.

    2016-01-01

    A biosensor platform based on Au/MXene nanocomposite for sensitive enzymatic glucose detection is reported. The biosensor leverages the unique electrocatalytic properties and synergistic effects between Au nanoparticles and MXene sheets. An amperometric glucose biosensor is fabricated by the immobilization of glucose oxidase (GOx) enzyme on Nafion solubilized Au/ MXene nanocomposite over glassy carbon electrode (GCE). The biomediated Au nanoparticles play a significant role in facilitating the electron exchange between the electroactive center of GOx and the electrode. The GOx/Au/MXene/Nafion/GCE biosensor electrode displayed a linear amperometric response in the glucose concentration range from 0.1 to 18 mM with a relatively high sensitivity of 4.2 μAmM−1 cm−2 and a detection limit of 5.9 μM (S/N = 3). Furthermore, the biosensor exhibited excellent stability, reproducibility and repeatability. Therefore, the Au/MXene nanocomposite reported in this work is a potential candidate as an electrochemical transducer in electrochemical biosensors.

  12. An Effective Amperometric Biosensor Based on Gold Nanoelectrode Arrays

    Directory of Open Access Journals (Sweden)

    Zhu Yingchun

    2008-01-01

    Full Text Available Abstract A sensitive amperometric biosensor based on gold nanoelectrode array (NEA was investigated. The gold nanoelectrode array was fabricated by template-assisted electrodeposition on general electrodes, which shows an ordered well-defined 3D structure of nanowires. The sensitivity of the gold NEA to hydrogen peroxide is 37 times higher than that of the conventional electrode. The linear range of the platinum NEA toward H2O2is from 1 × 10−6to 1 × 10−2 M, covering four orders of magnitudes with detection limit of 1 × 10−7 M and a single noise ratio (S/N of four. The enzyme electrode exhibits an excellent response performance to glucose with linear range from 1 × 10−5to 1 × 10−2 M and a fast response time within 8 s. The Michaelis–Menten constantkm and the maximum current densityi maxof the enzyme electrode were 4.97 mM and 84.60 μA cm−2, respectively. This special nanoelectrode may find potential application in other biosensors based on amperometric signals.

  13. Amperometric immunosensor for rapid detection of Mycobacterium tuberculosis

    International Nuclear Information System (INIS)

    Hiraiwa, Morgan; Lee, Hyun-Boo; Inoue, Shinnosuke; Chung, Jae-Hyun; Kim, Jong-Hoon; Becker, Annie L; Weigel, Kris M; Cangelosi, Gerard A; Lee, Kyong-Hoon

    2015-01-01

    Tuberculosis (TB) has been a major public health problem, which can be better controlled by using accurate and rapid diagnosis in low-resource settings. A simple, portable, and sensitive detection method is required for point-of-care (POC) settings. This paper studies an amperometric biosensor using a microtip immunoassay for a rapid and low-cost detection of Mycobacterium tuberculosis (MTB) in sputum. MTB in sputum is specifically captured on the functionalized microtip surface and detected by electric current. According to the numerical study, the current signal on the microtip surface is linearly changed with increasing immersion depth. Using a reference microtip, the immersion depth is compensated for a sensing microtip. On the microtip surface, target bacteria are concentrated and organized by a coffee-ring effect, which amplifies the electric current. To enhance the signal-to-noise ratio, both the sample processing and rinsing steps are presented with the use of deionized water as a medium for the amperometric measurement. When applied to cultured MTB cells spiked into human sputum, the detection limit was 100 CFU mL −1 , comparable to a more labor-intensive fluorescence detection method reported previously. (paper)

  14. Amperometric immunosensor for rapid detection of Mycobacterium tuberculosis

    Science.gov (United States)

    Hiraiwa, Morgan; Kim, Jong-Hoon; Lee, Hyun-Boo; Inoue, Shinnosuke; Becker, Annie L.; Weigel, Kris M.; Cangelosi, Gerard A.; Lee, Kyong-Hoon; Chung, Jae-Hyun

    2015-05-01

    Tuberculosis (TB) has been a major public health problem, which can be better controlled by using accurate and rapid diagnosis in low-resource settings. A simple, portable, and sensitive detection method is required for point-of-care (POC) settings. This paper studies an amperometric biosensor using a microtip immunoassay for a rapid and low-cost detection of Mycobacterium tuberculosis (MTB) in sputum. MTB in sputum is specifically captured on the functionalized microtip surface and detected by electric current. According to the numerical study, the current signal on the microtip surface is linearly changed with increasing immersion depth. Using a reference microtip, the immersion depth is compensated for a sensing microtip. On the microtip surface, target bacteria are concentrated and organized by a coffee-ring effect, which amplifies the electric current. To enhance the signal-to-noise ratio, both the sample processing and rinsing steps are presented with the use of deionized water as a medium for the amperometric measurement. When applied to cultured MTB cells spiked into human sputum, the detection limit was 100 CFU mL-1, comparable to a more labor-intensive fluorescence detection method reported previously.

  15. [Amperometric biosensor for ethanol analysis in wines and grape must during wine fermentation].

    Science.gov (United States)

    Shkotova, L V; Slast'ia, E A; Zhyliakova, T A; Soldatkin, O P; Schuhmann, W; Dziadevych, S V

    2005-01-01

    The amperometric biosensor for ethanol determination based on alcohol oxidase immobilised by the method of electrochemical polymerization has been developed. The industrial screen-printed platinum electrodes were used as transducers for creation of amperometric alcohol biosensor. Optimal conditions for electrochemical deposition of an active membrane with alcohol oxidase has been determined. Biosensors are characterised by good reproducibility and operational stability with minimal detection limit of ethanol 8 x 10(-5) M. The good correlation of results for ethanol detection in wine and during wine fermentation by using the developed amperometric biosensor with the data obtained by the standard methods was shown (r = 0.995).

  16. Flow Injection Analysis

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    1998-01-01

    Learning objectives:* To provide an introduction to automated assays* To describe the basic principles of FIA * To demonstrate the capabilities of FIA in relation to batch assays and conventional continuous flow systems* To show that FIA allows one to augment existing analytical techniques* To sh...... how FIA offers novel analytical procedures which are not feasible by conventional means* To hightlight the potentials of FIA in selected practical assays...

  17. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil); Santos, Clarissa M.M. dos; Flores, Erico M.M. [Departamento de Quimica Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Pozebon, Dirce, E-mail: dircepoz@iq.ufrgs.br [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil)

    2012-01-13

    Highlights: Black-Right-Pointing-Pointer Ultrasound was investigated and applied for red wine samples preparation. Black-Right-Pointing-Pointer Aliquots of 50 {mu}L of sample were nebulized and transported to plasma. Black-Right-Pointing-Pointer FI and pneumatic nebulization/aerosol desolvation were used. Black-Right-Pointing-Pointer LODs of the ICP-MS method for lanthanides determination were at ng L{sup -1} level. Black-Right-Pointing-Pointer Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 {mu}L of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L{sup -1}, respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  18. Surface-enhanced Raman detection of RNA and DNA bases following flow-injection analysis or HPLC separation

    Science.gov (United States)

    Cotton, Therese M.; Sheng, Rong-Sheng; Ni, Fan

    1990-11-01

    The goal of this study is to develop Surface-enhanced Raman scattering (SERS) detection methods for flow injection analysis (FIA) and high performance liquid chromatography (HPLC). Nucleic acid bases have been chosen for analysis because of their importance in life processes. The advantages to the use of SERS-based detection include its sensitivity, specificity and versatility. With the development of improved methodology, the detection limits should be comparable to UV spectroscopy. However, the specificity is considerably superior to that obtained with electronic spectroscopy in that the Raman spectrum provides a molecular fingerprint of the individual analytes. Raman spectroscopy is very versatile: aqueous samples, gases and solids can be analyzed with equal facility. The results presented here demonstrate that SERS can be used as a detection method for both FIA and HPLC detection. In the following experiments Ag sols have been used as the active substrate. The effect of various parameters such as temperature, pH, flow rate, and the nature of the interface between the HPLC system and the Raman spectrometer have been examined. One of the most significant findings is that the temperature of the Ag sol/HPLC effluent mixture has a dramatic effect on the SERS intensities. This effect is a result of increased colloid aggregation at higher temperatures. Aggregation is known to produce greater enhancement in SERS and proceeds much more rapidly at elevated temperatures. An increase in the temperature of the Ag sol enables SERS detection under flowing conditions and in real time. This is a substantial improvement over many of the previous attempts to interface SERS detection to FIA or HPLC. In most of the previous studies, it was necessary to stop the flow as the analyte eluted from the chromatogram and measure the SERS spectra under static conditions.

  19. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Santos, Clarissa M.M. dos; Flores, Érico M.M.; Pozebon, Dirce

    2012-01-01

    Highlights: ► Ultrasound was investigated and applied for red wine samples preparation. ► Aliquots of 50 μL of sample were nebulized and transported to plasma. ► FI and pneumatic nebulization/aerosol desolvation were used. ► LODs of the ICP-MS method for lanthanides determination were at ng L −1 level. ► Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L −1 , respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  20. Multicommuted flow injection method for fast photometric determination of phenolic compounds in commercial virgin olive oil samples.

    Science.gov (United States)

    Lara-Ortega, Felipe J; Sainz-Gonzalo, Francisco J; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2016-01-15

    A multicommuted flow injection method has been developed for the determination of phenolic species in virgin olive oil samples. The method is based on the inhibitory effect of antioxidants on a stable and colored radical cation formation from the colorless compound N,N-dimethyl-p-phenylenediamine (DMPD(•+)) in acidic medium in the presence of Fe(III) as oxidant. The signal inhibition by phenolic species and other antioxidants is proportional to their concentration in the olive oil sample. Absorbance was recorded at 515nm by means of a modular fiber optic spectrometer. Oleuropein was used as the standard for phenols determination and 6-hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (trolox) was the reference standard used for total antioxidant content calculation. Linear response was observed within the range of 250-1000mg/kg oleuropein, which was in accordance with phenolic contents observed in commercial extra virgin olive oil in the present study. Fast and low-volume liquid-liquid extraction of the samples using 60% MeOH was made previous to their insertion in the flow multicommuted system. The five three-way solenoid valves used for multicommuted liquid handling were controlled by a homemade electronic interface and Java-written software. The proposed approach was applied to different commercial extra virgin olive oil samples and the results were consistent with those obtained by the Folin Ciocalteu (FC) method. Total time for the sample preparation and the analysis required in the present approach can be drastically reduced: the throughput of the present analysis is 8 samples/h in contrast to 1sample/h of the conventional FC method. The present method is easy to implement in routine analysis and can be regarded as a feasible alternative to FC method. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Flow injection on-line oxidizing fluorometry coupled to dialysis sampling for the study of carbamazepine-protein binding

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhiqi [School of Chemistry and Materials Science, Shaanxi Normal University, Xi' an 710062 (China)]. E-mail: zqzhang@snnu.edu.cn; Liang Guoxi [School of Chemistry and Materials Science, Shaanxi Normal University, Xi' an 710062 (China)

    2005-04-22

    The mechanism of binding of carbamazepine (CBZ) with bovine serum albumin (BSA) has been investigated in vitro based on a new flow injection fluorometry coupled to the technique of dialysis sampling. The CBZ and BSA were mixed in different molar ratios in 0.050 mol L{sup -1} phosphate buffer (containing 0.9% NaCl), pH 7.4, and incubated at 37 {+-} 0.5 deg. C in a water bath. The dialysis sampler was utilized to sample free CBZ from mixed solution with a relative dialytic efficiency of 7.6%. Then the CBZ in dialysis solution was injected into carrier and on-line oxidized by lead dioxide solid-phase reactor into fluorescent product with a maximum excitation wavelength of 355 nm and a maximum emission wavelength of 478 nm. The fluorescence intensity measured was linear proportional with the concentration of free CBZ in mixed solution over the range of 1 x 10{sup -5} to 2 x 10{sup -4} mol L{sup -1} with the detection limit of 6 x 10{sup -6} mol L{sup -1}. According to the fluorescence measurement results from mixed solution, the association constant (K) estimated for CBZ-BSA binding and the number of the binding site (n) with Scatchard analysis were 1.08 x 10{sup 4} L mol{sup -1} and 0.94, respectively. Stern-Volmer plots indicated the presence of dynamic component in the quenching mechanism. The acting force was suggested to be mainly hydrophobic and the distance between the acceptor and donor was 3.12 nm. The estimated binding parameters agreed well with literature values.

  2. Flow-injection analysis of nitrate by reduction to nitrite and gas-phase molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Haghighi, B.; Tavassoli, A. [Dept. of Chemistry, Inst. for Advanced Studies in Basic Sciences, Zanjan (Iran)

    2001-12-01

    Two flow-injection manifolds have been investigated for the determination of nitrate. These manifolds are based on the reduction of nitrate to nitrite and determination of nitrite by gas-phase molecular absorption spectrophotometry. Nitrate sample solution (300 {mu}L) which is injected to the flow line, is reduced to nitrite by reaction with hydrazine or passage through the on-line copperized cadmium (Cd-Cu) reduction column. The nitrite produced reacts with a stream of hydrochloric acid and the evolved gases are purged into the stream of O{sub 2}carrier gas. The gaseous phase is separated from the liquid phase using a gas-liquid separator and then swept into a flow-through cell which has been positioned in the cell compartment of an UV-visible spectrophotometer. The absorbance of the gaseous phase is measured at 204.7 nm. A linear relationship was obtained between the intensity of absorption signals and concentration of nitrate when Cd-Cu reduction method was used, but a logarithmic relationship was obtained when the hydrazine reduction method was used. By use of the Cd-Cu reduction method, up to 330 {mu}g of nitrate was determined. The limit of detection was 2.97 {mu}g nitrate and the relative standard deviations for the determination of 12.0, 30.0 and 150 {mu}g nitrate were 3.32, 3.87 and 3.6%, respectively. Maximum sampling rate was approximately 30 samples per hour. The Cd-Cu reduction method was applied to the determination of nitrate and the simultaneous determination of nitrate and nitrite in meat products, vegetables, urine, and a water sample. (orig.)

  3. Flow-injection determination of total organic fluorine with off-line defluorination reaction on a solid sorbent bed.

    Science.gov (United States)

    Musijowski, Jacek; Trojanowicz, Marek; Szostek, Bogdan; da Costa Lima, José Luis Fontes; Lapa, Rui; Yamashita, Hiroki; Takayanagi, Toshio; Motomizu, Shoji

    2007-09-26

    Considering recent reports on widespread occurrence and concerns about perfluoroalkyl substances (PFAS) in environmental and biological systems, analysis of these compounds have gained much attention in recent years. Majority of analyte-specific methods are based on a LC/MS/MS or a GC/MS detection, however many environmental or biological studies would benefit from a total organic fluorine (TOF) determination. Presented work was aimed at developing a method for TOF determination. TOF is determined as an amount of inorganic fluoride obtained after defluorination reaction conducted off-line using sodium biphenyl reagent directly on the sorbent without elution of retained analytes. Recovered fluoride was analyzed using flow-injection system with either fluorimetric or potentiometric detection. The TOF method was tested using perfluorocarboxylic acids (PFCA), including perfluorooctanoic acid (PFOA), as model compounds. Considering low concentrations of PFAS in natural samples, solid-phase extraction as a preconcentration procedure was evaluated. Several carbon-based sorbents were tested, namely multi-wall carbon nanotubes, carbon nanofibres and activated carbon. Good sorption of all analytes was achieved and defluorination reaction was possible to carry out directly on a sorbent bed. Recoveries obtained for PFCAs, adsorbed on an activated carbon sorbent, and measured as TOF, were 99.5+/-1.7, 110+/-9.4, 95+/-26, 120+/-32, 110+/-12 for C4, C6, C8, C10 and C12-PFCA, respectively. Two flow systems that would enable the defluorination reaction and fluoride determination in a single system were designed and tested.

  4. Amperometric Determination of Glucose at Parts per Million Levels with Immobilized Glucose Oxidase.

    Science.gov (United States)

    Sittampalam, G.; Wilson, G. S.

    1982-01-01

    An experiment on the operation and utility of an amperometric immobilized enzyme electrode (or probe) is described, including advantages of the experiment, equipment, reagents, preparation of phosphate buffer, enzyme immobilization techniques, laboratory procedures, precautions, and discussion of experimental results. (SK)

  5. Evaluation of permselective membranes for optimization of intracerebral amperometric glutamate biosensors

    NARCIS (Netherlands)

    Wahono, N.; Qin, S.; Oomen, P.; Cremers, T. I. F.; de Vries, M. G.; Westerink, B. H. C.

    2012-01-01

    Monitoring of extracellular brain glutamate concentrations by intracerebral biosensors is a promising approach to further investigate the role of this important neurotransmitter. However, amperometric biosensors are typically hampered by Faradaic interference caused by the presence of other

  6. The procedure of ethanol determination in wine by enzyme amperometric biosensor

    Directory of Open Access Journals (Sweden)

    Dzyadevych S. V.

    2009-08-01

    Full Text Available Aim. Development of the procedure of ethanol determination in wine by an enzyme amperometric biosensor. Methods. The amperometric biosensor method of ethanol analysis has been used in this work. Results. The paper presents comparative analysis of two methods of alcohol oxidase (AO immobilization for development of amperometric biosensor for ethanol determination in wine. The method of AO immobilization in glutaraldehyde vapour was chosen as optimal for this purpose. The selectivity, operational and storage stability, and pH-optimum for operation of the created biosensor were determined. The procedure of ethanol determination in wine by amperometric biosensor on the basis of platinum printed electrode SensLab and AO was optimized. The analysis of ethanol concentration in wine and must samples was carried out using the developed high-stable biosensor. A good correlation between the data obtained by the biosensor and densitometry methods was shown. Conclusion. The proposed method of ethanol analysis could be used in wine production

  7. Modelling of Amperometric Biosensor Used for Synergistic Substrates Determination

    Directory of Open Access Journals (Sweden)

    Dainius Simelevicius

    2012-04-01

    Full Text Available In this paper the operation of an amperometric biosensor producing a chemically amplified signal is modelled numerically. The chemical amplification is achieved by using synergistic substrates. The model is based on non-stationary reaction-diffusion equations. The model involves three layers (compartments: a layer of enzyme solution entrapped on the electrode surface, a dialysis membrane covering the enzyme layer and an outer diffusion layer which is modelled by the Nernst approach. The equation system is solved numerically by using the finite difference technique. The biosensor response and sensitivity are investigated by altering the model parameters influencing the enzyme kinetics as well as the mass transport by diffusion. The biosensor action was analyzed with a special emphasis to the effect of the chemical amplification. The simulation results qualitatively explain and confirm the experimentally observed effect of the synergistic substrates conversion on the biosensor response.

  8. Integration of amperometric sensors for microchip capillary electrophoresis application

    International Nuclear Information System (INIS)

    Dicorato, F; Moore, E; Glennon, J

    2011-01-01

    Capillary electrophoresis is a technique for the separation and analysis of chemical compounds. Techniques adopted from the microchip technology knowledge have led to recent developments of electrophoresis system with integration on microchip. Microchip Capillary Electrophoresis (μCE) systems offer a series of advantages as easy integration for Lab-on-a-chip applications, high performance, portability, speed, minimal solvent and sample requirements. A new technological challenge aims at the development of an economic modular microchip capillary electrophoresis systems using separable and independent units concerning the sensor. In this project we worked on the development of an interchangeable amperometric sensor in order to provide a solution to such electrode passivation and facilitating the use of tailored sensors for specific analyte detection besides. Fluidic chips have been machined from cyclic olefin polymer pallets (Zeonor) using a micro-injection molding machine.

  9. Amperometric and impedance monitoring systems for biomedical applications

    CERN Document Server

    Punter-Villagrasa, Jaime; del Campo, Francisco J; Miribel, Pere

    2017-01-01

    The book presents the conception and realization of a pervasive electronic architecture for electrochemical applications, focusing on electronic instrumentation design and device development, particularly in electrochemical Point-of-Care and Lab-on-a-Chip devices, covering examples based on amperometric (DC) and impedance detection (AC) techniques. The presented electronics combine tailored front-end instrumentation and back-end data post-processing, enabling applications in different areas, and across a variety of techniques, analytes, transducers and environments. It addresses how the electronics are designed and implemented with special interest in the flow process: starting from electronic circuits and electrochemical biosensor design to a final validation and implementation for specific applications. Similarly, other important aspects are discussed throughout the book, such as electrochemical techniques, different analytes, targets, electronics reliability and robustness. The book also describes the use ...

  10. A flow-type amperometric sensor in immunoenzyme analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ivnitskii, D.M.; Aronbaev, D.M.; Kashkin, A.P.; Meringova, L.F.; Yulaev, M.F.

    1986-06-01

    A portable flow-type amperometric sensor has been made for the immunoenzyme determination of L-asparaginase. The authors show it is possible to determine peroxidase (the marker enzyme) by this method over the concentration range 1.10/sup -11/-4.10/sup -10/ M. The limit of detection for L-asparaginase is 1.8.10/sup -10/ M, which corresponds to clinically significant enzyme concentrations. Various modifications of immunoenzyme analysis (IEA) are used in clinical and research laboratories, and have contributed to diagnosis as regards antigens and serum antibodies. The sensor used here uses the electrical reduction of the molecular ion at the surface of thr measurement electrode. The electrochemical reaction is preceded by a competing antigen-antibody reaction and by the peroxidase oxidation of the iodide in the depressions.

  11. A Printed Organic Circuit System for Wearable Amperometric Electrochemical Sensors.

    Science.gov (United States)

    Shiwaku, Rei; Matsui, Hiroyuki; Nagamine, Kuniaki; Uematsu, Mayu; Mano, Taisei; Maruyama, Yuki; Nomura, Ayako; Tsuchiya, Kazuhiko; Hayasaka, Kazuma; Takeda, Yasunori; Fukuda, Takashi; Kumaki, Daisuke; Tokito, Shizuo

    2018-04-23

    Wearable sensor device technologies, which enable continuous monitoring of biological information from the human body, are promising in the fields of sports, healthcare, and medical applications. Further thinness, light weight, flexibility and low-cost are significant requirements for making the devices attachable onto human tissues or clothes like a patch. Here we demonstrate a flexible and printed circuit system consisting of an enzyme-based amperometric sensor, feedback control and amplification circuits based on organic thin-film transistors. The feedback control and amplification circuits based on pseudo-CMOS inverters were successfuly integrated by printing methods on a plastic film. This simple system worked very well like a potentiostat for electrochemical measurements, and enabled the quantitative and real-time measurement of lactate concentration with high sensitivity of 1 V/mM and a short response time of a hundred seconds.

  12. Measurement system for nitrous oxide based on amperometric gas sensor

    Science.gov (United States)

    Siswoyo, S.; Persaud, K. C.; Phillips, V. R.; Sneath, R.

    2017-03-01

    It has been well known that nitrous oxide is an important greenhouse gas, so monitoring and control of its concentration and emission is very important. In this work a nitrous oxide measurement system has been developed consisting of an amperometric sensor and an appropriate lab-made potentiostat that capable measuring picoampere current ranges. The sensor was constructed using a gold microelectrode as working electrode surrounded by a silver wire as quasi reference electrode, with tetraethyl ammonium perchlorate and dimethylsulphoxide as supporting electrolyte and solvent respectively. The lab-made potentiostat was built incorporating a transimpedance amplifier capable of picoampere measurements. This also incorporated a microcontroller based data acquisition system, controlled by a host personal computer using a dedicated computer program. The system was capable of detecting N2O concentrations down to 0.07 % v/v.

  13. Potentiometric and amperometric titration of ferrocene by cerium(4)

    International Nuclear Information System (INIS)

    Solomatin, V.T.

    1985-01-01

    Redox-potentials (E) of ferrocene (ferricenium-cation), Ce(4)/Ce(3) pairs are investigated and a possibility of regulating E value of these systems depending on the composition of water-organic media is shown. E value of Ce(4)/Ce(3) system decreases as increasing H 2 SO 4 concentration and CH 3 COOH mol share in the water-organic phase. Kinetic investigations of Ce(4)-ferrocene reactions shown that E constant value is achieved in 12-16 s depending on donor-acceptor properties of the solvent. Optimum conditions are chosen for potentiometric and amperometric titration of ferrocene by ceruium (4) in technological products. The method is versatile and permits to determine from tenths to dozens per cent of ferrocene

  14. Amperometric micro pH measurements in oxygenated saliva.

    Science.gov (United States)

    Chaisiwamongkhol, Korbua; Batchelor-McAuley, Christopher; Compton, Richard G

    2017-07-24

    An amperometric micro pH sensor has been developed based on the chemical oxidation of carbon fibre surfaces (diameter of 9 μm and length of ca. 1 mm) to enhance the population of surface quinone groups for the measurement of salivary pH. The pH analysis utilises the electrochemically reversible two-electron, two-proton behaviour of surface quinone groups on the micro-wire electrodes. A Nernstian response is observed across the pH range 2-8 which is the pH range of many biological fluids. We highlight the measurement of pH in small volumes of biological fluids without the need for oxygen removal and specifically the micro pH electrode is examined by measuring the pH of commercial synthetic saliva and authentic human saliva samples. The results correspond well with those obtained by using commercial glass pH electrodes on large volume samples.

  15. Integration of amperometric sensors for microchip capillary electrophoresis application

    Energy Technology Data Exchange (ETDEWEB)

    Dicorato, F; Moore, E [Life Sciences Interface Group, Tyndall National Institute, Lee Maltings, Dyke Parade, Cork (Ireland); Glennon, J, E-mail: eric.moore@tyndall.ie [Chemistry Department, University College Cork, College Road, Cork (Ireland)

    2011-08-17

    Capillary electrophoresis is a technique for the separation and analysis of chemical compounds. Techniques adopted from the microchip technology knowledge have led to recent developments of electrophoresis system with integration on microchip. Microchip Capillary Electrophoresis ({mu}CE) systems offer a series of advantages as easy integration for Lab-on-a-chip applications, high performance, portability, speed, minimal solvent and sample requirements. A new technological challenge aims at the development of an economic modular microchip capillary electrophoresis systems using separable and independent units concerning the sensor. In this project we worked on the development of an interchangeable amperometric sensor in order to provide a solution to such electrode passivation and facilitating the use of tailored sensors for specific analyte detection besides. Fluidic chips have been machined from cyclic olefin polymer pallets (Zeonor) using a micro-injection molding machine.

  16. Development of an automated technique for the speciation of arsenic using flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Ruede, T.R. (Inst. of Petrography and Geochemistry, Univ. of Karlsruhe (Germany)); Puchelt, H. (Inst. of Petrography and Geochemistry, Univ. of Karlsruhe (Germany))

    1994-09-01

    An automated method for the determination of arsenic acid (AsV), arsenous acid (AsIII), monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) was developed using a commercial available flow injection hydride generation system. By carrying out the hydride generation in selected acid media the determination of As(III) alone, of MMAA and DMAA by sum and by different sensitivities, and of all four species is possible. (orig.)

  17. Application of a novel metabolomic approach based on atmospheric pressure photoionization mass spectrometry using flow injection analysis for the study of Alzheimer's disease.

    Science.gov (United States)

    González-Domínguez, Raúl; García-Barrera, Tamara; Gómez-Ariza, José Luis

    2015-01-01

    The use of atmospheric pressure photoionization is not widespread in metabolomics, despite its considerable potential for the simultaneous analysis of compounds with diverse polarities. This work considers the development of a novel analytical approach based on flow injection analysis and atmospheric pressure photoionization mass spectrometry for rapid metabolic screening of serum samples. Several experimental parameters were optimized, such as type of dopant, flow injection solvent, and their flows, given that a careful selection of these variables is mandatory for a comprehensive analysis of metabolites. Toluene and methanol were the most suitable dopant and flow injection solvent, respectively. Moreover, analysis in negative mode required higher solvent and dopant flows (100 µl min(-1) and 40 µl min(-1), respectively) compared to positive mode (50 µl min(-1) and 20 µl min(-1)). Then, the optimized approach was used to elucidate metabolic alterations associated with Alzheimer's disease. Thereby, results confirm the increase of diacylglycerols, ceramides, ceramide-1-phosphate and free fatty acids, indicating membrane destabilization processes, and reduction of fatty acid amides and several neurotransmitters related to impairments in neuronal transmission, among others. Therefore, it could be concluded that this metabolomic tool presents a great potential for analysis of biological samples, considering its high-throughput screening capability, fast analysis and comprehensive metabolite coverage. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Evaluation of Flow-Injection Tandem Mass Spectrometry for Rapid and High-Throughput Quantitative Determination of B-Vitamins in Nutritional Supplements

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Deepak [ORNL; Van Berkel, Gary J [ORNL

    2012-01-01

    The use of flow-injection electrospray ionization tandem mass spectrometry for rapid and high-throughput mass spectral analysis of selected B-vitamins, viz. B1, B2, B3, B5, and B6, in nutritional formulations was demonstrated. A simple and rapid (~5 min) in-tube sample preparation was performed by adding extraction solvent to a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Automated flow injection introduced 1 L of the extracts directly into the mass spectrometer ion source without chromatographic separation. Sample-to-sample analysis time was 60 s representing significant improvement over conventional liquid chromatography approaches which typically require 25-45 min, and often require more significant sample preparation procedures. Quantitative capabilities of the flow-injection analysis were tested using the method of standard additions and NIST standard reference material (SRM 3280) multivitamin/multielement tablets. The quantity determined for each B-vitamin in SRM 3280 was within the statistical range provided for the respective certified values. The same sample preparation and analysis approach was also applied to two different commercial vitamin supplement tablets and proved to be successful in the quantification of the selected B-vitamins as evidenced by an agreement with the labels values and the results obtained using isotope dilution liquid chromatography/mass spectrometry.

  19. Ionophore-Based Potentiometric Sensors for the Flow-Injection Determination of Promethazine Hydrochloride in Pharmaceutical Formulations and Human Urine

    Directory of Open Access Journals (Sweden)

    Suad Mustafa Al-Araji

    2011-01-01

    Full Text Available Plasticised poly(vinyl chloride-based membranes containing the ionophores (α-, β- and γ-cyclodextrins (CD, dibenzo-18-crown-6 (DB18C6 and dibenzo-30-crown-10 (DB30C10 were evaluated for their potentiometric response towards promethazine (PM in a flow injection analysis (FIA set-up. Good responses were obtained when β- and γ-CDs, and DB30C10 were used. The performance characteristics were further improved when tetrakis(4-chlorophenyl borate (KTPB was added to the membrane. The sensor based on β-CD, bis(2-ethylhexyl adipate (BEHA and KTPB exhibited the best performance among the eighteen sensor compositions that were tested. The response was linear from 1 x 10−5 to 1 x 10−2 M, slope was 61.3 mV decade−1, the pH independent region ranged from 4.5 to 7.0, a limit of detection of 5.3 x 10−6 M was possible and a lifetime of more than a month was observed when used in the FIA system. Other plasticisers such as dioctyl phenylphosphonate and tributyl phosphate do not show significant improvements in the quality of the sensors. The promising sensors were further tested for the effects of foreign ions (Li+, Na+, K+, Mg2+, Ca2+, Co2+, Cu2+, Cr3+, Fe3+, glucose, fructose. FIA conditions (e.g., effects of flow rate, injection volume, pH of the carrier stream were also studied when the best sensor was used (based on β-CD. The sensor was applied to the determination of PM in four pharmaceutical preparations and human urine that were spiked with different levels of PM. Good agreement between the sensor and the manufacturer’s claimed values (for pharmaceutical preparations was obtained, while mean recoveries of 98.6% were obtained for spiked urine samples. The molecular recognition features of the sensors as revealed by molecular modelling were rationalised by the nature of the interactions and complexation energies between the host and guest molecules.

  20. Establish an automated flow injection ESI-MS method for the screening of fragment based libraries: Application to Hsp90.

    Science.gov (United States)

    Riccardi Sirtori, Federico; Caronni, Dannica; Colombo, Maristella; Dalvit, Claudio; Paolucci, Mauro; Regazzoni, Luca; Visco, Carlo; Fogliatto, Gianpaolo

    2015-08-30

    ESI-MS is a well established technique for the study of biopolymers (nucleic acids, proteins) and their non covalent adducts, due to its capacity to detect ligand-target complexes in the gas phase and allows inference of ligand-target binding in solution. In this article we used this approach to investigate the interaction of ligands to the Heat Shock Protein 90 (Hsp90). This enzyme is a molecular chaperone involved in the folding and maturation of several proteins which has been subjected in the last years to intensive drug discovery efforts due to its key role in cancer. In particular, reference compounds, with a broad range of dissociation constants from 40pM to 100μM, were tested to assess the reliability of ESI-MS for the study of protein-ligand complexes. A good agreement was found between the values measured with a fluorescence polarization displacement assay and those determined by mass spectrometry. After this validation step we describe the setup of a medium throughput screening method, based on ESI-MS, suitable to explore interactions of therapeutic relevance biopolymers with chemical libraries. Our approach is based on an automated flow injection ESI-MS method (AFI-MS) and has been applied to screen the Nerviano Medical Sciences proprietary fragment library of about 2000 fragments against Hsp90. In order to discard false positive hits and to discriminate those of them interacting with the N-terminal ATP binding site, competition experiments were performed using a reference inhibitor. Gratifyingly, this group of hits matches with the ligands previously identified by NMR FAXS techniques and confirmed by X-ray co-crystallization experiments. These results support the use of AFI-MS for the screening of medium size libraries, including libraries of small molecules with low affinity typically used in fragment based drug discovery. AFI-MS is a valid alternative to other techniques with the additional opportunities to identify compounds interacting with

  1. Flow injection on-line dilution for zinc determination in human saliva with electrothermal atomic absorption spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Burguera-Pascu, Margarita [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain)], E-mail: margaburpas@hotmail.com; Rodriguez-Archilla, Alberto [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain); Burguera, Jose Luis; Burguera, Marcela; Rondon, Carlos; Carrero, Pablo [Department of Chemistry, Faculty of Sciences, University of Los Andes, Merida (Venezuela)

    2007-09-26

    An automated method is described for the determination of zinc in human saliva by electrothermal atomic absorption spectrometry (ET AAS) after on-line dilution of samples with a significant reduction of sample consumption per analysis (<0.4 mL including the dead volume of the system). In order to fulfill this aim without changing the sample transport conduits during the experiments, a flow injection (FI) dilution system was constructed. Its principal parts are: one propulsion device (peristaltic pump, PP) for either samples, standards or washing solution all located in an autosampler tray and for the surfactant solution (Triton X-100) used as diluent, and a two-position time based solenoid injector (TBSI{sub 1}) which allowed the introduction of 10 {mu}L of either solution in the diluent stream. To avoid unnecessary waste of samples, the TBSI{sub 1} also permitted the recirculation of the solutions to their respective autosampler cups. The downstream diluted solution fills a home made sampling arm assembly. The sequential deposition of 20 {mu}L aliquots of samples or standards on the graphite tube platform was carried out by air displacement with a similar time based solenoid injector (TBSI{sub 2}). The dilution procedure and the injection of solutions into the atomizer are computer controlled and synchronized with the operation of the temperature program. Samples or standards solutions were submitted to two drying steps (at 90 and 130 deg. C), followed by pyrolysis and atomization at 700 and 1700 deg. C, respectively. The aqueous calibration was linear up to 120.0 {mu}g L{sup -1} for diluted standard solutions/samples and its slope was similar (p > 0.05) to the standard addition curve, indicating lack of matrix effect. The precision tested by repeated analysis of real saliva samples was less than 3% and the detection limit (3{sigma}) was of 0.35 {mu}g L{sup -1}. To test the accuracy of the proposed procedure, recovery tests were performed, obtaining mean recovery

  2. Construction and performance characterization of ion-selective electrodes for potentiometric determination of pseudoephedrine hydrochloride applying batch and flow injection analysis techniques.

    Science.gov (United States)

    Zayed, Sayed I M; Issa, Yousry M; Hussein, Ahmed

    2006-01-01

    New pseudoephedrine selective electrodes have been constructed of the conventional polymer membrane type by incorporation of pseudoephedrine-phosphotungstate (PE-PT) or pseudoephedrine-silicotungstate (PE-SiT) ion-associates in a poly vinyl chloride (PVC) membrane plasticized with dibutyl phthalate (DBP). The electrodes were fully characterized in terms of the membrane composition, temperature, and pH. The electrodes exhibited mean slopes of calibration graphs of 57.09 and 56.10 mV concentration decade(-1) of PECl at 25 degrees C for (PE-PT) and (PE-SiT) electrodes, respectively. The electrodes showed fast, stable, and near-Nernstian response over the concentration ranges 6.31 x 10(-6)-1.00 x 10(-2) and 5.00 x 10(-5)-1.00x10(-2) M in the case of PE-PT applying batch and flow injection (FI) analysis, respectively, and 1.00 x 10(-5)-1.00 x 10(-2) and 5.00 x 10(-5)-1.00x10(-2) M in the case of PE-SiT for batch and FI analysis system, respectively. Detection limit was 5.01x 10(-6) M for PE-PT electrode and 6.31x10(-6) M for PE-SiT electrode. The electrodes were successfully applied for the potentiometric determination of pseudoephedrine hydrochloride (PECl) in pharmaceutical preparations with mean recovery 101.13 +/- 0.85% and 100.77+0.79% in case of PE-PT applying batch and flow injection systems, respectively, and 100.75+0.85% and 100.79 +/- 0.77% in case of PE-SiT for batch and flow injection systems, respectively. The electrodes exhibited good selectivity for PECl with respect to a large number of inorganic cations, sugars and amino acids.

  3. Rapid food decomposition by H2O2-H2SO4 for determination of total mercury by flow injection cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Zenebon, Odair; Sakuma, Alice M; Dovidauskas, Sergio; Okada, Isaura A; de, MaioFrancaD; Lichtig, Jaim

    2002-01-01

    A mixture of 50% H2O2-H2SO4 (3 + 1, v/v) was used for decomposition of food in open vessels at 80 degrees C. The treatment allowed rapid total mercury determination by flow injection cold vapor atomic absorption spectrometry. Cabbage, potatoes, peanuts paste, hazelnuts paste, oats, tomatoes and their derivatives, oysters, shrimps, prawns, shellfish, marine algae, and many kinds of fish were analyzed by the proposed methodology with a limit of quantitation of 0.86 +/- 0.08 microg/L mercury in the final solution. Reference materials tested also gave excellent recovery.

  4. Rapid isolation of biomarkers for compound specific radiocarbon dating using high-performance liquid chromatography and flow injection analysis-atmospheric pressure chemical ionisation mass spectrometry.

    Science.gov (United States)

    Smittenberg, Rienk H; Hopmans, Ellen C; Schouten, Stefan; Sinninghe Damsté, Jaap S

    2002-11-29

    Repeated semi-preparative normal-phase HPLC was performed to isolate selected biomarkers from sediment extracts for radiocarbon analysis. Flow injection analysis-mass spectrometry was used for rapid analysis of collected fractions to evaluate the separation procedure, taking only 1 min per fraction. In this way 100-1000 microg of glycerol dialkyl glycerol tetraethers, sterol fractions and chlorophyll-derived phytol were isolated from typically 100 g of marine sediment, i.e., in sufficient quantities for radiocarbon analysis, without significant carbon isotopic fractionation or contamination.

  5. Improvement of amperometric transducer selectivity using nanosized phenylenediamine films

    Science.gov (United States)

    Soldatkina, O. V.; Kucherenko, I. S.; Pyeshkova, V. M.; Alekseev, S. A.; Soldatkin, O. O.; Dzyadevych, S. V.

    2017-11-01

    In this work, we studied the conditions of deposition of a semipermeable polyphenylenediamine (PPD)-based membrane on amperometric disk platinum electrodes. Restricting an access of interfering substances to the electrode surface, the membrane prevents their impact on the sensor operation. Two methods of membrane deposition by electropolymerization were compared—at varying potential (cyclic voltammetry) and at constant potential. The cyclic voltammetry was shown to be easier in performing and providing better properties of the membrane. The dependence of PPD membrane effectiveness on the number of cyclic voltammograms and phenylenediamine concentration was analyzed. It was shown that the impact of interfering substances (ascorbic acid, dopamine, cysteine, uric acid) on sensor operation could be completely avoided using three cyclic voltammograms in 30 mM phenylenediamine. On the other hand, when working with diluted samples, i.e., at lower concentrations of electroactive substances, it is reasonable to decrease the phenylenediamine concentration to 5 mM, which would result in a higher sensitivity of transducers to hydrogen peroxide due to a thinner PPD layer. The PPD membrane was tested during continuous operation and at 8-day storage and turned out to be efficient in sensor and biosensors.

  6. Construction of ferrocene modified conducting polymer based amperometric urea biosensor.

    Science.gov (United States)

    Dervisevic, Muamer; Dervisevic, Esma; Senel, Mehmet; Cevik, Emre; Yildiz, Huseyin Bekir; Camurlu, Pınar

    2017-07-01

    Herein, an electrochemical urea sensing bio-electrode is reported that has been constructed by firstly electropolymerizing 4-(2,5-Di(thiophen-2-yl)-1H-pyrrol-1-yl)aniline monomer (SNS-Aniline) on Pencil Graphite Electrode (PGE), then modifying the polymer coated electrode surface with di-amino-Ferrocene (DAFc) as the mediator, and lastly Urease enzyme through glutaraldehyde crosslinking. The effect of pH, temperature, polymer thickness, and applied potential on the electrode current response was investigated besides performing storage and operational stability experiments with the interference studies. The resulting urea biosensor's amperometric response was linear in the range of 0.1-8.5mM with the sensitivity of 0.54μA/mM, detection limit of 12μM, and short response time of 2s. The designed bio-electrode was tested with real human blood and urine samples where it showed excellent analytical performance with insignificant interference. Copyright © 2017 Elsevier Inc. All rights reserved.

  7. Pencil graphite leads as simple amperometric sensors for microchip electrophoresis.

    Science.gov (United States)

    Natiele Tiago da Silva, Eiva; Marques Petroni, Jacqueline; Gabriel Lucca, Bruno; Souza Ferreira, Valdir

    2017-11-01

    In this work we demonstrate, for the first time, the use of inexpensive commercial pencil graphite leads as simple amperometric sensors for microchip electrophoresis. A PDMS support containing one channel was fabricated through soft lithography and sanded pencil graphite leads were inserted into this channel to be used as working electrodes. The electrochemical and morphological characterization of the sensor was carried out. The graphite electrode was coupled to PDMS microchips in end-channel configuration and electrophoretic experiments were performed using nitrite and ascorbate as probe analytes. The analytes were successfully separated and detected in well-defined peaks with satisfactory resolution using the microfluidic platform proposed. The repeatability of the pencil graphite electrode was satisfactory (RSD values of 1.6% for nitrite and 12.3% for ascorbate, regarding the peak currents) and its lifetime was estimated to be ca. 700 electrophoretic runs over a cost of ca. $ 0.05 per electrode. The limits of detection achieved with this system were 2.8 μM for nitrite and 5.7 μM for ascorbate. For proof of principle, the pencil graphite electrode was employed for the real analysis of well water samples and nitrite was successfully quantified at levels below its maximum contaminant level established in Brazil and US. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A new amperometric enzyme electrode for alcohol determination.

    Science.gov (United States)

    Gülce, H; Gülce, A; Kavanoz, M; Coşkun, H; Yildiz, A

    2002-06-01

    A new enzyme electrode for the determination of alcohols was developed by immobilizing alcohol oxidase in polvinylferrocenium matrix coated on a Pt electrode surface. The amperometric response due to the electrooxidation of enzymatically generated H(2)O(2) was measured at a constant potential of +0.70 V versus SCE. The effects of substrate, buffer and enzyme concentrations, pH and temperature on the response of the electrode were investigated. The optimum pH was found to be pH 8.0 at 30 degrees C. The steady-state current of this enzyme electrode was reproducible within +/-5.0% of the relative error. The sensitivity of the enzyme electrode decreased in the following order: methanol>ethanol>n-butanol>benzyl alcohol. The linear response was observed up to 3.7 mM for methanol, 3.0 mM for ethanol, 6.2 mM for n-butanol, and 5.2 mM for benzyl alcohol. The apparent Michaelis-Menten constant (K(Mapp)) value and the activation energy, E(a), of this immobilized enzyme system were found to be 5.78 mM and 38.07 kJ/mol for methanol, respectively.

  9. Spatially and time-resolved element-specific in situ corrosion investigations with an online hyphenated microcapillary flow injection inductively coupled plasma mass spectrometry set-up

    International Nuclear Information System (INIS)

    Homazava, N.; Ulrich, A.; Kraehenbuehl, U.

    2008-01-01

    A novel technique for in situ spatial, time-resolved element-specific investigations of corrosion processes is developed. The technique is based on an online hyphenation of a specially designed microflow-capillary set-up to inductively coupled plasma mass spectrometry (ICP-MS) using flow injection sample introduction. Detailed aspects of the method development, optimization of the sample microflow introduction and flow injection characteristics for the localized corrosion analysis are described. Moreover, specific challenges of the ICP-MS analysis as applied to the analysis of corrosion sample probes, e.g. high matrix load and limited sample volume, are discussed. The efficiency of the developed technique is proved by corrosion susceptibility analysis of a commercial Al alloy. Results of the corrosion experiments of the aluminum alloy AA 6111 are presented to demonstrate the influence of various factors such as exposure time and pH value of the corrosive medium on the element-specific dissolution rates of the alloy. This novel technique provides new aspects in corrosion science and sheds new light on corrosion mechanisms

  10. Simultaneous Determination of Iron, Copper and Cobalt in Food Samples by CCD-diode Array Detection-Flow Injection Analysis with Partial Least Squares Calibration Model

    International Nuclear Information System (INIS)

    Mi Jiaping; Li Yuanqian; Zhou Xiaoli; Zheng Bo; Zhou Ying

    2006-01-01

    A flow injection-CCD diode array detection spectrophotometry with partial least squares (PLS) program for simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction of the three metal ions and 2- (5-Bromo-2-pyridylazo)-5-diethylaminophenol, 5-Br-PADAP in acetic acid - sodium acetate buffer solution (pH5) with Triton X-100 and ascorbic acid. The overlapped spectra of the colored complexes were collected by charge-coupled device (CCD) - diode array detector and the multi-wavelength absorbance data was processed using partial least squares (PLS) algorithm. Optimum reaction conditions and parameters of flow injection analysis were investigated. The samples of tea, sesame, laver, millet, cornmeal, mung bean and soybean powder were determined by the proposed method. The average recoveries of spiked samples were 91.80%∼100.9% for Iron, 92.50%∼108.0% for Copper, 93.00%∼110.5% for Cobalt, respectively with relative standard deviation (R.S.D) of 1.1%∼12.1%. The sampling rate is 45 samples h -1 . The determination results of the food samples were in good agreement between the proposed method and ICP-AES

  11. Simultaneous Determination of Iron, Copper and Cobalt in Food Samples by CCD-diode Array Detection-Flow Injection Analysis with Partial Least Squares Calibration Model

    Energy Technology Data Exchange (ETDEWEB)

    Mi Jiaping; Li Yuanqian; Zhou Xiaoli; Zheng Bo; Zhou Ying [West China School of Public Health, Sichuan University, Chengdu, 610041 (China)

    2006-01-01

    A flow injection-CCD diode array detection spectrophotometry with partial least squares (PLS) program for simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction of the three metal ions and 2- (5-Bromo-2-pyridylazo)-5-diethylaminophenol, 5-Br-PADAP in acetic acid - sodium acetate buffer solution (pH5) with Triton X-100 and ascorbic acid. The overlapped spectra of the colored complexes were collected by charge-coupled device (CCD) - diode array detector and the multi-wavelength absorbance data was processed using partial least squares (PLS) algorithm. Optimum reaction conditions and parameters of flow injection analysis were investigated. The samples of tea, sesame, laver, millet, cornmeal, mung bean and soybean powder were determined by the proposed method. The average recoveries of spiked samples were 91.80%{approx}100.9% for Iron, 92.50%{approx}108.0% for Copper, 93.00%{approx}110.5% for Cobalt, respectively with relative standard deviation (R.S.D) of 1.1%{approx}12.1%. The sampling rate is 45 samples h{sup -1}. The determination results of the food samples were in good agreement between the proposed method and ICP-AES.

  12. Simultaneous Determination of Iron, Copper and Cobalt in Food Samples by CCD-diode Array Detection-Flow Injection Analysis with Partial Least Squares Calibration Model

    Science.gov (United States)

    Mi, Jiaping; Li, Yuanqian; Zhou, Xiaoli; Zheng, Bo; Zhou, Ying

    2006-01-01

    A flow injection-CCD diode array detection spectrophotometry with partial least squares (PLS) program for simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction of the three metal ions and 2- (5-Bromo-2-pyridylazo)-5-diethylaminophenol, 5-Br-PADAP in acetic acid - sodium acetate buffer solution (pH5) with Triton X-100 and ascorbic acid. The overlapped spectra of the colored complexes were collected by charge-coupled device (CCD) - diode array detector and the multi-wavelength absorbance data was processed using partial least squares (PLS) algorithm. Optimum reaction conditions and parameters of flow injection analysis were investigated. The samples of tea, sesame, laver, millet, cornmeal, mung bean and soybean powder were determined by the proposed method. The average recoveries of spiked samples were 91.80%~100.9% for Iron, 92.50%~108.0% for Copper, 93.00%~110.5% for Cobalt, respectively with relative standard deviation (R.S.D) of 1.1%~12.1%. The sampling rate is 45 samples h-1. The determination results of the food samples were in good agreement between the proposed method and ICP-AES.

  13. Quantitative Analysis of Piroxicam Using Temperature-Controlled Ionic Liquid Dispersive Liquid Phase Microextraction Followed By Stopped-Flow Injection Spectrofluorimetry

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Ganjali

    2013-07-01

    Full Text Available Background:Piroxicam (PXM belongs to the wide class of non-steroidal anti-inflammatory drugs (NSAIDs. PXM has been widely applied in the treatment of rheumatoid arthritis, gonarthrosis, osteoarthritis, backaches, neuralgia, mialgia. In the presented work, a green and benign sample pretreatment method called temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was followed with stopped-flow injection spectrofluorimetry (SFIS for quantitation of PXM in pharmaceutical formulations and biological samples.Methods:Temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was applied as an environmentally friendly sample enrichment method to extract and isolate PXM prior to quantitation. Dispersion of 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF6] ionic liquid (IL through the sample aqueous solution was performed by applying a relatively high temperature. PXM was extracted into the extractor, and after phase separation, PXM in the final solution was determined by stopped-flow injection spectrofluorimetry (SFIS.Results and Major Conclusion:Different factors affecting the designed method such as IL amount, diluting agent, pH and temperature were investigated in details and optimized. The method provided a linear dynamic range of 0.2-150 μg l-1, a limit of detection (LOD of 0.046 μg l-1 and a relative standard deviation (RSD of 3.1%. Furthermore, in order to demonstrate the analytical applicability of the recommended method, it was applied for quantitation of PXM in real samples.

  14. A Simple and Rapid Flow-Injection Chemiluminescence Method for the Determination of Noscapine with Ru(phen)32+-Ce(4) System

    International Nuclear Information System (INIS)

    Rezaei, B.; Mokhtari, A.; Khayamian, T.

    2007-01-01

    A new flow injection chemiluminescence (CL) system was used for the determination of noscapine. This technique is based on the reduction effect of noscapine on the Ru(phen) 3 3+ , which is produced by reaction between Ru(phen) 3 2+ and acidic Ce(4) solutions, and this rapid reduction produces strong CL. Calibration plots were linear over the range of 3.0x10 -7 -2.0x10 -6 mol L -1 and 2.0x10 -6 -2.0x10 -4 mol L -1 . The CL intensity was so high, that it is able to produce a detection limit of 6.6x10 -8 M noscapine (3σ). The relative standard deviation of 2.0x10 -6 M noscapine was 1.0% (n=10). The proposed method was successfully applied for the flow injection determination of noscapine in cough and Tonin syrup samples. The results of real sample analyses show good recovery percentages (97.3-102.4%). The minimum sampling rate was 100 samples per hour

  15. AN APPLICATION OF FLOW INJECTION ANALYSIS WITH GAS DIFFUSION AND SPECTROPHOTOMETRIC DETECTION FOR THE MONITORING OF DISSOLVED SULPHIDE CONCENTRATION IN ENVIRONMENTAL SAMPLES

    Directory of Open Access Journals (Sweden)

    Malwina Cykowska

    2014-10-01

    Full Text Available The monitoring of the concentration of sulphide is very important from the environment point of view because of high toxicity of hydrogen sulphide. What is more hydrogen sulphide is an important pollution indicator. In many cases the determination of sulphide is very difficult due to complicated matrix of some environmental samples, which causes that most analytical methods cannot be used. Flow injection analysis allows to avoid matrix problem what makes it suitable for a wide range of applications in analytical laboratories. In this paper determination of dissolved sulphide in environmental samples by gas-diffusion flow injection analysis with spectrophotometric detection was presented. Used gas-diffusion separation ensures the elimination of interferences caused by sample matrix and gives the ability of determination of sulphides in coloured and turbid samples. Studies to optimize the measurement conditions and to determine the value of the validation parameters (e.g. limit of detection, limit of quantification, precision, accuracy were carried out. Obtained results confirm the usefulness of the method for monitoring the concentration of dissolved sulphides in water and waste water. Full automation and work in a closed system greatly reduces time of analysis, minimizes consumption of sample and reagents and increases safety of analyst’s work.

  16. On-line monitoring of glucose and/or lactate in a fermentation process using an expanded micro-bed flow injection analyser.

    Science.gov (United States)

    Nandakumar, M P; Lali, A M; Mattiasson, B

    1999-01-01

    A novel flow injection biosensor system for monitoring fermentation processes has been developed using an expanded micro bed as the enzyme reactor. An expanded bed reactor is capable of handling a mobile phase containing suspended matter like cells and cell debris. Thus, while the analyte is free to interact with the adsorbent, the suspended particulate matter passes through unhindered. With the use of a scaled down expanded bed in the flow injection analysis (FIA) system, it was possible to analyse samples directly from a fermentor without the pretreatment otherwise required to extract the analyte or remove the suspended cells. This technique, therefore, provides a means to determine the true concentrations of the metabolites in a fermentor, with more ease than possible with other techniques. Glucose oxidase immobilised on STREAMLINE was used to measure glucose concentration in a suspension of dead yeast cells. There was no interference from the cell particles even at high cell densities such as 15 gm dry weight per litre. The assay time was about 6 min. Accuracy and reproducibility of the system was found to be good. In another scheme, lactate oxidase was covalently coupled to STREAMLINE for expanded bed operation. With the on-line expanded micro bed FIA it was possible to follow the fermentation with Lactobacillus casei.

  17. Reengineered glucose oxidase for amperometric glucose determination in diabetes analytics.

    Science.gov (United States)

    Arango Gutierrez, Erik; Mundhada, Hemanshu; Meier, Thomas; Duefel, Hartmut; Bocola, Marco; Schwaneberg, Ulrich

    2013-12-15

    Glucose oxidase is an oxidoreductase exhibiting a high β-D-glucose specificity and high stability which renders glucose oxidase well-suited for applications in diabetes care. Nevertheless, GOx activity is highly oxygen dependent which can lead to inaccuracies in amperometric β-D-glucose determinations. Therefore a directed evolution campaign with two rounds of random mutagenesis (SeSaM followed by epPCR), site saturation mutagenesis studies on individual positions, and one simultaneous site saturation library (OmniChange; 4 positions) was performed. A diabetes care well suited mediator (quinone diimine) was selected and the GOx variant (T30V I94V) served as starting point. For directed GOx evolution a microtiter plate detection system based on the quinone diimine mediator was developed and the well-known ABTS-assay was applied in microtiter plate format to validate oxygen independency of improved GOx variants. Two iterative rounds of random diversity generation and screening yielded to two subsets of amino acid positions which mainly improved activity (A173, A332) and oxygen independency (F414, V560). Simultaneous site saturation of all four positions with a reduced subset of amino acids using the OmniChange method yielded finally variant V7 with a 37-fold decreased oxygen dependency (mediator activity: 7.4 U/mg WT, 47.5 U/mg V7; oxygen activity: 172.3 U/mg WT, 30.1 U/mg V7). V7 is still highly β-D-glucose specific, highly active with the quinone diimine mediator and thermal resistance is retained (prerequisite for GOx coating of diabetes test stripes). The latter properties and V7's oxygen insensitivity make V7 a very promising candidate to replace standard GOx in diabetes care applications. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Carbon coated magnesium oxide based amperometric glucose biosensor

    Energy Technology Data Exchange (ETDEWEB)

    Silva, L.L.; Mello, J.M.M.; Fiori, M.A.; Duarte, G.W. [Universidade Comunitaria Regional de Chapeco (UNICHAPECO), SC (Brazil); Fernandes, S.C. [Instituto Federal Catarinense (IFC), Blumenau, SC (Brazil); Riella, H.G. [Centro Universitario Barriga Verde (UNIBAVE), Orleans, SC (Brazil); Anzolin, C.; Figueiro, A.; Grando, M.C. [Universidade Federal de Santa Catarina (UFSC), SC (Brazil)

    2016-07-01

    Full text: Diabetes is a serious disease that is harmful to human health since it is related to cardiovascular and stroke events. Since the first glucose oxidase (GOx) sensor, different approaches have been explored. Carbon was used to cover nano-magnesium oxide (MgO-C) forming a core-shell which was used to improve its biocompatibility and chemical stability for the preparation of GOx biosensor. MgO nanostructures have been prepared by calcination of the gel formed by the reaction of magnesium acetate tetrahydrate dissolved in cetyltrimethylammonium with the addition of tartaric acid solution. MgO-C nanostructures were obtained by heating MgO nanoparticles previously prepared together with glucose and PEG dissolved in an aqueous suspension. Reaction conditions such as concentration of magnesium precursor, temperature and aging time show important roles in the size, morphology and growth process of the final products. The core-shell structure was evidenced by SEM/FEG and XRD and showed that the product appeared to have morphological forms of nanowires. GOx was spread onto the surface of a modified carbon paste electrode (CPE) doped with MgO-C and the effect on the biosensing properties investigated by comparing the electrochemical properties of the proposed biosensor with bare and modified CPEs by cyclic voltammetry. The amount of modifier in CPE (5-75 weight% with respect to graphite) influences the peak current and the influence of different experimental parameters (enzyme percentage, pH solution and amperometric methods) was also investigated. The results demonstrate that the GOx retains its biocatalytic activity and that the bioelectrode modified can be a possible use for other nanotechnological purposes including biomedical ones. (author)

  19. Development of a Telemetric, Miniaturized Electrochemical Amperometric Analyzer.

    Science.gov (United States)

    Jung, Jaehyo; Lee, Jihoon; Shin, Siho; Kim, Youn Tae

    2017-10-23

    In this research, we developed a portable, three-electrode electrochemical amperometric analyzer that can transmit data to a PC or a tablet via Bluetooth communication. We performed experiments using an indium tin oxide (ITO) glass electrode to confirm the performance and reliability of the analyzer. The proposed analyzer uses a current-to-voltage (I/V) converter to convert the current generated by the reduction-oxidation (redox) reaction of the buffer solution to a voltage signal. This signal is then digitized by the processor. The configuration of the power and ground of the printed circuit board (PCB) layer is divided into digital and analog parts to minimize the noise interference of each part. The proposed analyzer occupies an area of 5.9 × 3.25 cm² with a current resolution of 0.4 nA. A potential of 0~2.1 V can be applied between the working and the counter electrodes. The results of this study showed the accuracy of the proposed analyzer by measuring the Ruthenium(III) chloride ( Ru III ) concentration in 10 mM phosphate-buffered saline (PBS) solution with a pH of 7.4. The measured data can be transmitted to a PC or a mobile such as a smartphone or a tablet PC using the included Bluetooth module. The proposed analyzer uses a 3.7 V, 120 mAh lithium polymer battery and can be operated for 60 min when fully charged, including data processing and wireless communication.

  20. Carbon coated magnesium oxide based amperometric glucose biosensor

    International Nuclear Information System (INIS)

    Silva, L.L.; Mello, J.M.M.; Fiori, M.A.; Duarte, G.W.; Fernandes, S.C.; Riella, H.G.; Anzolin, C.; Figueiro, A.; Grando, M.C.

    2016-01-01

    Full text: Diabetes is a serious disease that is harmful to human health since it is related to cardiovascular and stroke events. Since the first glucose oxidase (GOx) sensor, different approaches have been explored. Carbon was used to cover nano-magnesium oxide (MgO-C) forming a core-shell which was used to improve its biocompatibility and chemical stability for the preparation of GOx biosensor. MgO nanostructures have been prepared by calcination of the gel formed by the reaction of magnesium acetate tetrahydrate dissolved in cetyltrimethylammonium with the addition of tartaric acid solution. MgO-C nanostructures were obtained by heating MgO nanoparticles previously prepared together with glucose and PEG dissolved in an aqueous suspension. Reaction conditions such as concentration of magnesium precursor, temperature and aging time show important roles in the size, morphology and growth process of the final products. The core-shell structure was evidenced by SEM/FEG and XRD and showed that the product appeared to have morphological forms of nanowires. GOx was spread onto the surface of a modified carbon paste electrode (CPE) doped with MgO-C and the effect on the biosensing properties investigated by comparing the electrochemical properties of the proposed biosensor with bare and modified CPEs by cyclic voltammetry. The amount of modifier in CPE (5-75 weight% with respect to graphite) influences the peak current and the influence of different experimental parameters (enzyme percentage, pH solution and amperometric methods) was also investigated. The results demonstrate that the GOx retains its biocatalytic activity and that the bioelectrode modified can be a possible use for other nanotechnological purposes including biomedical ones. (author)

  1. Development of a Telemetric, Miniaturized Electrochemical Amperometric Analyzer

    Directory of Open Access Journals (Sweden)

    Jaehyo Jung

    2017-10-01

    Full Text Available In this research, we developed a portable, three-electrode electrochemical amperometric analyzer that can transmit data to a PC or a tablet via Bluetooth communication. We performed experiments using an indium tin oxide (ITO glass electrode to confirm the performance and reliability of the analyzer. The proposed analyzer uses a current-to-voltage (I/V converter to convert the current generated by the reduction-oxidation (redox reaction of the buffer solution to a voltage signal. This signal is then digitized by the processor. The configuration of the power and ground of the printed circuit board (PCB layer is divided into digital and analog parts to minimize the noise interference of each part. The proposed analyzer occupies an area of 5.9 × 3.25 cm2 with a current resolution of 0.4 nA. A potential of 0~2.1 V can be applied between the working and the counter electrodes. The results of this study showed the accuracy of the proposed analyzer by measuring the Ruthenium(III chloride ( Ru III concentration in 10 mM phosphate-buffered saline (PBS solution with a pH of 7.4. The measured data can be transmitted to a PC or a mobile such as a smartphone or a tablet PC using the included Bluetooth module. The proposed analyzer uses a 3.7 V, 120 mAh lithium polymer battery and can be operated for 60 min when fully charged, including data processing and wireless communication.

  2. A flow-through amperometric sensor based on dialysis tubing and free enzyme reactors

    NARCIS (Netherlands)

    Bohm, S.; Pijanowska, D.G.; Pijanowska, D.; Olthuis, Wouter; Bergveld, Piet

    2001-01-01

    A generic flow-through amperometric microenzyme sensor is described, which is based on semi-permeable dialysis tubing carrying the sample to be analyzed. This tubing (300 μm OD) is led through a small cavity, containing the working and reference electrode. By filling this cavity with a few μl of an

  3. Increasing amperometric biosensor sensitivity by length fractionated single-walled carbon nanotubes

    DEFF Research Database (Denmark)

    Tasca, Federico; Gorton, Lo; Wagner, Jakob Birkedal

    2008-01-01

    In this work the sensitivity-increasing effect of single-walled carbon nanotubes (SWCNTs) in amperometric biosensors, depending on their average length distribution, was studied. For this purpose the SWCNTs were oxidatively shortened and subsequently length separated by size exclusion...

  4. Flow-injection determination of thorium and uranium after on-line ion-exchange preconcentration in Dowex 50-X8

    International Nuclear Information System (INIS)

    Perez Pavon, J.L.; Garcia Pinto, C.G.; Rodriguez Garcia, Estrella; Moreno Cordero, Bernardo

    1992-01-01

    The preconcentration of thorium and uranium on Dowex 50-X8 was studied as a method for the preconcentration of these cations prior to their determination by flow injection with spectrophotometric detection using Arsenazo III in 3.6 M HCl stabilized with Triton X-100 as chromogenic reagent. The preconcentration device is a minicolumn included in the sample loop of the injection valve. A second valve contains a reducing minicolumn filled with lead powder to reduce U(VI) to U(IV) before the confluence of the sample with the reagent stream. The method can be applied to samples containing 0.5-100 μg l -1 and was tested with different spiked water samples. (author). 15 refs.; 3 figs.; 3 tabs

  5. Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of cyanide using cadmium carbonate as a new solid-phase reactor

    International Nuclear Information System (INIS)

    Noroozifar, M.; Khorasani-Motlagh, M.; Hosseini, S.-N.

    2005-01-01

    A new and simple flow injection system procedure has been developed for the indirect determination of cyanide. The method is based on insertion of aqueous cyanide solutions into an on-line cadmium carbonate packed column (25% m/m suspended on silica gel beads) and a sodium hydroxide with pH 10 is used as the carrier stream. The eluent containing the analyte as cadmiumcyanide complexes, produced from reaction between cadmium carbonate and cyanide, measured by flame atomic absorption spectrometry. The absorbance is proportional to the concentration of cyanide in the sample. The linear range of the system is up to 15 mg L -1 with a detection limit 0.2 mg L -1 and sampling rate 72 h -1 . The method is suitable for determination of cyanide in industrial waste waters with a relative standard deviation better than 1.22%

  6. Characterization of organic and conventional sweet basil leaves using chromatographic and flow-injection mass spectrometric (FIMS) fingerprints combined with principal component analysis

    Science.gov (United States)

    Lu, Yingjian; Gao, Boyan; Chen, Pei; Charles, Denys; Yu, Liangli (Lucy)

    2014-01-01

    Sweet basil, Ocimum basilicum., is one of the most important and wildly used spices and has been shown to have antioxidant, antibacterial, and anti-diarrheal activities. In this study, high performance liquid chromatographic (HPLC) and flow-injection mass spectrometric (FIMS) fingerprinting techniques were used to differentiate organic and conventional sweet basil leaf samples. Principal component analysis (PCA) of the fingerprints indicated that both HPLC and FIMS fingerprints could effectively detect the chemical differences in the organic and conventional sweet basil leaf samples. This study suggested that the organic basil sample contained greater concentrations of almost all the major compounds than its conventional counterpart on a per same botanical weight basis. The FIMS method was able to rapidly differentiate the organic and conventional sweet basil leaf samples (1 min analysis time), whereas the HPLC fingerprints provided more information about the chemical composition of the basil samples with a longer analytical time. PMID:24518341

  7. Determination of uranium in natural waters and high-purity aluminum by flow-injection on-line preconcentration and ICP-MS detection

    International Nuclear Information System (INIS)

    Seki, Tatsuya; Oguma, Koichi

    2004-01-01

    A flow injection method has been developed for the determination of uranium is natural waters and high-purity aluminum by use of on-line preconcentration on a U/TEVA TM column and ICP-MS detection. The sample solution prepared as a nitric acid solution in 3 mol l -1 was passed through the U/TEVA TM column to collect uranium and uranium adsorbed was eluted with 0.1 mol l -1 nitric acid. The effluent was introduced directly into the nebulizer of the ICP-MS and 238 U was measured. The detection limit, calculated as 3-times the standard deviation of the background noise, was 3pg and the sample throughput was about 10 per hour. The proposed method was successfully applied to the determination of uranium in river-water reference materials, a seawater reference material and high-purity aluminum reference materials. (author)

  8. The Use of Flow-Injection Analysis with Chemiluminescence Detection of Aqueous Ferrous Iron in Waters Containing High Concentrations of Organic Compounds

    Directory of Open Access Journals (Sweden)

    Carrick M. Eggleston

    2009-06-01

    Full Text Available An evaluation of flow-injection analysis with chemiluminescence detection (FIA-CL to quantify Fe2+(aq in freshwaters was performed. Iron-coordinating and/or iron-reducing compounds, dissolved organic matter (DOM, and samples from two natural water systems were used to amend standard solutions of Fe2+(aq. Slopes of the response curves from ferrous iron standards (1 – 100 nM were compared to the response curves of iron standards containing the amendments. Results suggest that FIA-CL is not suitable for systems containing ascorbate, hydroxylamine, cysteine or DOM. Little or no change in sensitivity occurred in solutions of oxalate and glycine or in natural waters with little organic matter.

  9. Flow Injection Potentiometric Determination of Cd2+ Ions Using a Coated Graphite Plasticized PVC-Membrane Electrode Based on 1, 3-Bis(2-cyanobenzene)triazene.

    Science.gov (United States)

    Shamsipur, Mojtaba; Sahari, Shokat; Payehghadr, Mahmood; Alizadeh, Kamal

    2011-09-01

    1, 3-Bis(2-cyanobenzene)triazene, L, was used as a suitable ionophore for the fabrication of a new PVC-based polymeric membrane coated graphite electrode for selective sensing of Cd2+ ion. The electrode exhibited a selective linear Nernstian response to Cd2+ ion at an optimal pH range of 6-9 with a limit of detection of 8.0 × 10-6 M and a fast response time of about 2 s. The electrode was used as a proper detection system in flow-injection potentiometry of cadmium ion and resulted in well defined peaks for cadmium ions with stable baseline, excellent reproducibility and high sampling rates of over 100 injections per hour. It showed good stability, reproducibility and fast response time. The practical utility of the proposed system has also been reported.

  10. Incorporation of flow injection analysis with dual-wavelength overlapping resonance Rayleigh scattering for rapid determination of malachite green and its metabolite in fish.

    Science.gov (United States)

    Zhu, Jinghui; Qin, Mingyou; Liu, Shaopu; Liu, Zhongfang; Yang, Jidong; Hu, Xiaoli

    2014-09-15

    A flow injection analysis (FIA) system combined with dual-wavelength overlapping resonance Rayleigh scattering (DWO-RRS) has been established and validated for rapid determination of malachite green (MG) and its metabolite in fish samples. Under experimental condition, MG would react with Erythrosin (Ery) to form ion-association complexes, resulting in the occurrence of two RRS peaks and a dramatic enhancement of RRS intensity. The maximum RRS peaks were located at 286 nm and 337 nm. It is noted that the increments of both of these two peaks were proportional to the concentration of MG. The detection limit of DWO-RRS was 1.5 ng/mL, which was comparable to several reported methods. Moreover, the results of real sample analysis exhibited an acceptable recovery between 97.5% and 103.6%, indicating that the method had good reproducibility. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Flow injection microfluidic device with on-line fluorescent derivatization for the determination of Cr(III) and Cr(VI) in water samples after solid phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Peng, Guilong [Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045 (China); Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, 100084 (China); He, Qiang, E-mail: heqiang0980@163.com [Key Laboratory of Eco-Environment of Three Gorges Region of Ministry of Education, Chongqing University, Chongqing, 400045 (China); Lu, Ying [Department of Mathematics and Physics, Armed Police College, Chengdu, 610213 (China); Huang, Jing [Research Center for Advanced Computation, College of Science, Xihua University, Chengdu, 610039 (China); Lin, Jin-Ming, E-mail: jmlin@mail.tsinghua.edu.cn [Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, 100084 (China)

    2017-02-22

    In this paper, a rapid and simple method using magnetic multi-walled carbon nanotubes (MWCNTS), as a solid-phase extraction (SPE) sorbent, was successfully developed for extraction and preconcentration trace amounts of Cr(III) in water samples. The synthesized magnetic-MWCNTs nanocomposite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). A rhodamine derivative (R1) was synthesized and characterized as a highly selective and sensitive fluorescent derivatizing agent for Cr(III). After SPE procedure, Cr(III) analysis was performed by flow injection microfluidic chip with on-line fluorescent derivatization and laser-induced fluorescence (LIF) spectroscopy detection. The parameters, which affected the efficiency of the developed method were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 0–10.0 nM, with a detection limit of 0.094 nM and an enrichment factor of 38. Furthermore, real water samples were analyzed and good recoveries were obtained from 91.0 to 101.6%. - Graphical abstract: Flow injection microfluidic device with on-line fluorescent derivatization and detection coupled to LIF. - Highlights: • A highly selective and sensitive derivatizing reagent for Cr(III) was synthesized and characterized. • The magnetic-MWCNTs nanocomposite as a SPE sorbent was successfully synthesized and characterized. • A new portable detection system was developed for microfluidic chip FIA platform.

  12. Chitosan-guar gum-silver nanoparticles hybrid matrix with immobilized enzymes for fabrication of beta-glucan and glucose sensing photometric flow injection system.

    Science.gov (United States)

    Bagal-Kestwal, Dipali R; Kestwal, Rakesh Mohan; Hsieh, Wen-Ting; Chiang, Been-Huang

    2014-01-01

    Simple and fast photometric flow injection analysis system was developed for sensing of β-1,3-glucan from medicinal mushroom Ganoderma lucidum during fermentation. For this purpose, the chitosan-guar gum-silver nanoparticle-beta glucanase (Ch-GG-AgNPs-βG) beads and Ch-GG-AgNPs-GOD (glucose oxidase) beads were prepared. The bead packed mini-columns were then used to assemble a flow injection analysis (FIA) system for the detection of β-(1→3)-d-glucan biomarker or glucose. This colorimetric flow system can detect glucose and glucan with detection limits as low as 50ngmL(-1) and 100ngmL(-1) (S/N=3), respectively. The analysis time of this FIA was approximately 40s, which is faster than the previously reported glucan sensors. The glucose and glucan calibration curves were obtained in the range of 0.25-1.25μgmL(-1) (R(2)=0.988) and 0.2-1.0μgmL(-1)(R(2)=0.979), respectively. The applicability of the nano-bio-composite FIA sensor system for spiked and real β-(1→3)-d-glucan samples were tested, and the accuracy of the results were greater than 95%. Thus, the designed FIA provides a simple, interference free and rapid tool for monitoring glucose and β-glucan content, which can be used for various food samples with a little modification. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Rapid Quantitation of Ascorbic and Folic Acids in SRM 3280 Multivitamin/Multielement Tablets using Flow-Injection Tandem Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bhandari, Deepak [ORNL; Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2013-01-01

    RATIONALE: Ascorbic acid (AA) and folic acid (FA) are water-soluble vitamins and are usually fortified in food and dietary supplements. For the safety of human health, proper intake of these vitamins is recommended. Improvement in the analysis time required for the quantitative determination of these vitamins in food and nutritional formulations is desired. METHODS: A simple and fast (~5 min) in-tube sample preparation was performed, independently for FA and AA, by mixing extraction solvent with a powdered sample aliquot followed by agitation, centrifugation, and filtration to recover an extract for analysis. Quantitative detection was achieved by flow-injection (1 L injection volume) electrospray ionization tandem mass spectrometry (ESI-MS/MS) in negative ion mode using the method of standard addition. RESULTS: Method of standard addition was employed for the quantitative estimation of each vitamin in a sample extract. At least 2 spiked and 1 non-spiked sample extract were injected in triplicate for each quantitative analysis. Given an injection-to-injection interval of approximately 2 min, about 18 min was required to complete the quantitative estimation of each vitamin. The concentration values obtained for the respective vitamins in the standard reference material (SRM) 3280 using this approach were within the statistical range of the certified values provided in the NIST Certificate of Analysis. The estimated limit of detections of FA and AA were 13 and 5.9 ng/g, respectively. CONCLUSIONS: Flow-injection ESI-MS/MS was successfully applied for the rapid quantitation of FA and AA in SRM 3280 multivitamin/multielement tablets.

  14. Elaboration of new method of enzyme adsorption on silicalite and nano beta zeolite for amperometric biosensor creation

    Directory of Open Access Journals (Sweden)

    Soldatkin O. O.

    2014-07-01

    Full Text Available Aim. Optimization of a new method of enzyme immobilization for amperometric biosensor creation. Methods. The amperometric biosensor with glucose oxidase immobilized on zeolites as bioselective elements and platinum disk electrode as transducers of biochemical signal into the electric one was used in the work. Results. The biosensors based on glucose oxidase adsorbed on zeolites were characterized by a higher sensitivity to glucose and a better inter-reproducibility. The best analytical characteristics were obtained for the biosensors based on nano beta zeolite. It has been found that an increase in the amount of zeolite on the surface of amperometric transducer may change such biosensor parameters as sensitivity to the substrate and duration of the analysis. Conclusions. The proposed method of enzyme immobilization by adsorption on zeolites is shown to be quite promising in the development of amperometric biosensors and therefore should be further investigated.

  15. Discrimination of Aurantii Fructus Immaturus and Fructus Poniciri Trifoliatae Immaturus by Flow Injection UV Spectroscopy (FIUV) and 1H NMR using Partial Least-squares Discriminant Analysis (PLS-DA)

    Science.gov (United States)

    Two simple fingerprinting methods, flow-injection UV spectroscopy (FIUV) and 1H nuclear magnetic resonance (NMR), for discrimination of Aurantii FructusImmaturus and Fructus Poniciri TrifoliataeImmaturususing were described. Both methods were combined with partial least-squares discriminant analysis...

  16. DIFFERENTIATION OF AURANTII FRUCTUS IMMATURUS AND FRUCTUS PONICIRI TRIFOLIATAE IMMATURUS BY FLOW-INJECTION WITH ULTRAVIOLET SPECTROSCOPIC DETECTION AND PROTON NUCLEAR MAGNETIC RESONANCE USING PARTIAL LEAST-SQUARES DISCRIMINANT ANALYSIS.

    Science.gov (United States)

    Zhang, Mengliang; Zhao, Yang; Harrington, Peter de B; Chen, Pei

    2016-03-01

    Two simple fingerprinting methods, flow-injection coupled to ultraviolet spectroscopy and proton nuclear magnetic resonance, were used for discriminating between Aurantii fructus immaturus and Fructus poniciri trifoliatae immaturus . Both methods were combined with partial least-squares discriminant analysis. In the flow-injection method, four data representations were evaluated: total ultraviolet absorbance chromatograms, averaged ultraviolet spectra, absorbance at 193, 205, 225, and 283 nm, and absorbance at 225 and 283 nm. Prediction rates of 100% were achieved for all data representations by partial least-squares discriminant analysis using leave-one-sample-out cross-validation. The prediction rate for the proton nuclear magnetic resonance data by partial least-squares discriminant analysis with leave-one-sample-out cross-validation was also 100%. A new validation set of data was collected by flow-injection with ultraviolet spectroscopic detection two weeks later and predicted by partial least-squares discriminant analysis models constructed by the initial data representations with no parameter changes. The classification rates were 95% with the total ultraviolet absorbance chromatograms datasets and 100% with the other three datasets. Flow-injection with ultraviolet detection and proton nuclear magnetic resonance are simple, high throughput, and low-cost methods for discrimination studies.

  17. Determination of As(III) and As(V) by Flow Injection-Hydride Generation-Atomic Absorption Spectrometry via On-line Reduction of As(V) by KI

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1997-01-01

    A volume-based flow injection (FI) procedure is described for the determination and speciation of trace inorganic arsenic, As(III) and As(V), via hydride generation-atomic absorption spectrometry (HG-AAS) of As(III). The determination of total arsenic is obtained by on-line reduction of As(V) to As...

  18. Functional materials in amperometric sensing polymeric, inorganic, and nanocomposite materials for modified electrodes

    CERN Document Server

    Seeber, Renato; Zanardi, Chiara

    2014-01-01

    Amperometric sensors, biosensors included, particularly rely on suitable electrode materials. Progress in material science has led to a wide variety of options that are available today. For the first time, these novel functional electrode coating materials are reviewed in this monograph, written by and for electroanalytical chemists. This includes intrinsically conducting, redox and ion-exchange polymers, metal and carbon nanostructures, silica based materials. Monolayers and relatively thick films are considered. The authors critically discuss preparation methods, in addition to chemical and

  19. A Reagentless Amperometric Formaldehyde-Selective Chemosensor Based on Platinized Gold Electrodes

    OpenAIRE

    Demkiv, Olha; Smutok, Oleh; Gonchar, Mykhailo; Nisnevitch, Marina

    2017-01-01

    Fabrication and characterization of a new amperometric chemosensor for accurate formaldehyde analysis based on platinized gold electrodes is described. The platinization process was performed electrochemically on the surface of 4 mm gold planar electrodes by both electrolysis and cyclic voltamperometry. The produced electrodes were characterized using scanning electron microscopy and X-ray spectral analysis. Using a low working potential (0.0 V vs. Ag/AgCl) enabled an essential increase in th...

  20. Amperometric biosensor for lactate analysis in wine and must during fermentation

    OpenAIRE

    Shkotova , L.V.; Goriushkina , T.B.; Tran-Minh , Canh; Chovelon , Jean-Marc; Soldatkin , A.P.; Dzyadevych , S.V.

    2008-01-01

    MADICA 2006 Conference, Fifth Maghreb-Europe Meeting on Materials and their Applicatons for Devices and Physical, Chemical and Biological Sensors, MADICA 2006 Conference, Fifth Maghreb-Europe Meeting on Materials and their Applicatons for Devices and Physical, Chemical and Biological Sensors; International audience; A lactate oxidase-based amperometric biosensor is designed for lactate determination. Two methods of lactate oxidase immobilization on the surface of commercial SensLab platinum p...

  1. Analogs of N-cynnamoylphenylhydroxylamine as reagents for amperometric determination of scandium

    International Nuclear Information System (INIS)

    Shvedene, N.V.; Gallaj, Z.A.; Sheina, N.M.; Zujkova, N.V.

    1978-01-01

    To decrease the detection limit of scandium and increase selectivity of amperometric determination, oxidation of 2-furylacryloyl-N-p-chlorophenylhydroxylamine (FACPhHA) and 3-styrylacryloyl-N-phenylhydroxylamine (SAPhHA) on a graphite electrode has been studied by volt-amperometry. The possibility has been established of using the oxidation current of the reagent for plotting the titration curves. The solubility of scandium complexes with FACPhHA and SAPhHA under conditions of titration against the background with pH 6.0 has been determined and equals (2.1+-0.3)x10 -6 and (5.3+-0.3)x10 -7 , respectively. The methods have been developed of amperometric determination of scandium with the use of the considered reagents against backgrounds with pH 5.5-6.5. The use of SAPhHA has decreased the limit of scandium detection down to 0.1 mgk/ml. Besides, the amperometric method makes it possible to titrate in turbid and coloured media what is an advantage of this method. The developed method is used for determination of scandium in scandium silicide

  2. Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

    2016-05-01

    High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

  3. Investigation of iron(III) reduction and trace metal interferences in the determination of dissolved iron in seawater using flow injection with luminol chemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Ussher, Simon J. [School of Earth, Ocean and Environmental Sciences (SEOES), University of Plymouth, Drake Circus, Plymouth PL4 8AA (United Kingdom); Milne, Angela [School of Earth, Ocean and Environmental Sciences (SEOES), University of Plymouth, Drake Circus, Plymouth PL4 8AA (United Kingdom); Department of Oceanography, Florida State University, Tallahassee, FL 32306-4320 (United States); Landing, William M. [Department of Oceanography, Florida State University, Tallahassee, FL 32306-4320 (United States); Attiq-ur-Rehman, Kakar [Department of Chemistry, University of Balochistan, Quetta (Pakistan); Seguret, Marie J.M.; Holland, Toby [School of Earth, Ocean and Environmental Sciences (SEOES), University of Plymouth, Drake Circus, Plymouth PL4 8AA (United Kingdom); Achterberg, Eric P. [National Oceanography Centre, University of Southampton, European Way, Southampton SO14 3ZH (United Kingdom); Nabi, Abdul [Department of Chemistry, University of Balochistan, Quetta (Pakistan); Worsfold, Paul J., E-mail: pworsfold@plymouth.ac.uk [School of Earth, Ocean and Environmental Sciences (SEOES), University of Plymouth, Drake Circus, Plymouth PL4 8AA (United Kingdom)

    2009-10-12

    A detailed investigation into the performance of two flow injection-chemiluminescence (FI-CL) manifolds (with and without a preconcentration column) for the determination of sub-nanomolar dissolved iron (Fe(II) + Fe(III)), following the reduction of Fe(III) by sulphite, in seawater is described. Kinetic experiments were conducted to examine the efficiency of reduction of inorganic Fe(III) with sulphite under different conditions and a rigorous study of the potential interference caused by other transition metals present in seawater was conducted. Using 100 {mu}M concentrations of sulphite a reduction time of 4 h was sufficient to quantitatively reduce Fe(III) in seawater. Under optimal conditions, cobalt(II) and vanadium(IV)/(III) were the major positive interferences and strategies for their removal are reported. Specifically, cobalt(II) was masked by the addition of dimethylglyoxime to the luminol solution and vanadium(IV) was removed by passing the sample through an 8-hydroxyquinoline column in a low pH carrier stream. Manganese(II) also interfered by suppression of the CL response but this was not significant at typical open ocean concentrations.

  4. A rapid and accurate method for determining protein content in dairy products based on asynchronous-injection alternating merging zone flow-injection spectrophotometry.

    Science.gov (United States)

    Liang, Qin-Qin; Li, Yong-Sheng

    2013-12-01

    An accurate and rapid method and a system to determine protein content using asynchronous-injection alternating merging zone flow-injection spectrophotometry based on reaction between coomassie brilliant blue G250 (CBBG) and protein was established. Main merit of our approach is that it can avoid interferences of other nitric-compounds in samples, such as melamine and urea. Optimized conditions are as follows: Concentrations of CBBG, polyvinyl alcohol (PVA), NaCl and HCl are 150 mg/l, 30 mg/l, 0.1 mol/l and 1.0% (v/v), respectively; volumes of the sample and reagent are 150 μl and 30 μl, respectively; length of a reaction coil is 200 cm; total flow rate is 2.65 ml/min. The linear range of the method is 0.5-15 mg/l (BSA), its detection limit is 0.05 mg/l, relative standard deviation is less than 1.87% (n=11), and analytical speed is 60 samples per hour. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Determination of boron in natural water and products derived from grape using an automated flow injection analysis system with piezoelectric detection

    International Nuclear Information System (INIS)

    Jesus, Dosil P. de; Saito, Renata M.; Lago, Claudimir L. do

    2004-01-01

    An automated flow injection analysis system with piezoelectric detection is proposed as a sensitive and selective method for boron. The detector is an electrode-separated piezoelectric quartz crystal coated with N-methyl-D-glucamine-modified poly(epichlorohydrin). The film ability to retain boron allows the adjustment of the linear dynamic range and the sensitivity by varying the injected sample volume. In the present work, the sample volumes were varied from 0.5 to 5.0 mL. Among several ionic species, germanate is the only one that can interfere in the method. Nevertheless, it can be eliminated by addition of sulfide to the sample. The method was successfully applied to the determination of boron concentration in samples of natural water (from 1.71 to 309 μL -1 ) and products derived from grape juice (from 2.06 to 6.21 mg L -1 ). A pretreatment with hydrogen peroxide in alkaline medium was required due to the great amount of sugars in the grape products (author)

  6. Manual and Flow-Injection Detection/Quantification of Polyquaterniums via Fully Reversible Polyion-Sensitive Polymeric Membrane-Based Ion-Selective Electrodes.

    Science.gov (United States)

    Ferguson, Stephen A; Meyerhoff, Mark E

    2017-10-27

    The detection of four different polyquaterniums (PQs) using a fully reversible potentiometric polyion sensor in three different detection modes is described. The polyion sensing "pulstrodes" serve as the detector for direct dose-response experiments, beaker titrations, and in a flow-injection analysis (FIA) system. Direct polycation response toward PQ-2, PQ-6, PQ-10, and poly(2-methacryloxyethyltrimethylammonium) chloride (PMETAC) yields characteristic information about each PQ species (e.g., relative charge densities, etc.) via syringe pump addition of each PQ species to a background electrolyte solution. Quantitative titrations are performed using a syringe pump to deliver heparin as the polyanion titrant to quantify all four PQs at μg/mL levels. Both the direct and indirect methods incorporate the use of a three-electrode system including counter, double junction reference, and working electrodes. The working electrode possesses a plasticized poly(vinyl chloride) (PVC) membrane containing the neutral lipophilic salt of dinonylnaphthalenesulfonate (DNNS - ) tridodecylmethylammonium (TDMA + ). Further, the titration method is shown to be useful to quantify PQ-6 levels in recreational swimming pool water collected in Ann Arbor, MI. Finally, a FIA system equipped with a pulstrode detector is used to demonstrate the ability to potentially quantify PQ levels via a more streamlined and semiautomated testing platform.

  7. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

    Science.gov (United States)

    Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

    2009-08-15

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 microl of 9.0 mol L(-1) hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3ngL(-1) and the relative standard deviation (RSD) for 10 replicates at 1 microg L(-1) Hg(2+) was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  8. Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Martinis, Estefania M.; Berton, Paula; Olsina, Roberto A.; Altamirano, Jorgelina C.; Wuilloud, Rodolfo G.

    2009-01-01

    A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 mim][PF 6 ]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 μl of 9.0 mol L -1 hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L -1 and the relative standard deviation (RSD) for 10 replicates at 1 μg L -1 Hg 2+ was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

  9. Determination of technetium-99, thorium-230 and uranium-234 in soils by inductively coupled plasma mass spectrometry using flow injection preconcentration

    International Nuclear Information System (INIS)

    Hollenbach, Mark; Grohs, James; Mamich, Stephen; Kroft, Marilyn; Denoyer, E.R.

    1994-01-01

    A new method is described for the determination of 99 Tc, 230 Th, and 234 U at ultra-trace levels in soils. The method used flow injection (FI) for on-line preconcentration of 99 Tc, 230 Th and 234 U prior to detection using inductively coupled plasma mass spectrometry (ICP-MS). The FI-ICP-MS method results in greater sensitivity and freedom from interferences compared with direct aspiration into an ICP mass spectrometer. Detection limits are improved by approximately a factor of 10. The FI-ICP-MS method is also faster, less labour intensive and generates less laboratory waste than traditional radiochemical methods. The accuracy of the method was tested for 99 Tc by comparison to liquid scintillation counting and for 230 Th and 234 U by analysis of a US Department of Energy reference soil. Detection limits in the soil for 99 Tc, 230 Th and 234 U were 11 mBq g -1 (0.02 ng g -1 ), 3.7 mBq g -1 (0.005 ng g -1 ) and 0.74 mBq g -1 (0.003 ng g -1 ), respectively. Sample preparation, analysis protocol, and method validation are described. (Author)

  10. Toward a high-throughput method for determining vicine and convicine levels in faba bean seeds using flow injection analysis combined with tandem mass spectrometry.

    Science.gov (United States)

    Purves, Randy W; Khazaei, Hamid; Vandenberg, Albert

    2018-08-01

    Although faba bean provides environmental and health benefits, vicine and convicine (v-c) limit its use as a source of vegetable protein. Crop improvement efforts to minimize v-c concentration require low-cost, rapid screening methods to distinguish between high and low v-c genotypes to accelerate development of new cultivars and to detect out-crossing events. To assist crop breeders, we developed a unique and rapid screening method that uses a 60 s instrumental analysis step to accurately distinguish between high and low v-c genotypes. The method involves flow injection analysis (FIA) coupled with tandem mass spectrometry (i.e., selective reaction monitoring, SRM). Using seeds with known v-c levels as calibrants, measured v-c levels were comparable with liquid chromatography (LC)-SRM results and the method was used to screen 370 faba bean genotypes. Widespread use of FIA-SRM will accelerate breeding of low v-c faba bean, thereby alleviating concerns about anti-nutritional effects of v-c in this crop. Copyright © 2018 Elsevier Ltd. All rights reserved.

  11. Highly sensitive determination of diclofenac based on resin beads and a novel polyclonal antibody by using flow injection chemiluminescence competitive immunoassay

    Science.gov (United States)

    Shi, Jing; Xu, Mingxia; Tang, Qinghui; Zhao, Kang; Deng, Anping; Li, Jianguo

    2018-02-01

    A novel flow injection chemiluminescence immunoassay for simple, sensitive and low-cost detection of diclofenac was established based on specific binding of antigen and antibody. Carboxylic resin beads used as solid phase carrier materials provided good biocompatibility and large surface-to-volume ratio for modifying more coating antigen. There was a competitive process between the diclofenac in solution and the immobilized coating antigen to react with the limited binding sites of the polyclonal antibody to form the immunocomplex. The second antibody labelled with horseradish peroxidase was introduced into the immunosensor and trapped by captured polyclonal antibody against diclofenac, which could effectively amplify chemiluminescence signals of luminol-PIP-H2O2. Under optimal conditions, the diclofenac could be detected quantitatively. The chemiluminescence intensity decreased linearly with the logarithm of the diclofenac concentration in the range of 0.1-100 ng mL- 1 with a detection limit of 0.05 ng mL- 1 at a signal-to-noise ratio of 3. The immunosensor exhibited high sensitivity, specificity and acceptable stability. This easy-operated and cost-effective analytical method could be valuable for the diclofenac determination in real water samples.

  12. Determination of scandium in acid mine drainage by ICP-OES with flow injection on-line preconcentration using oxidized multiwalled carbon nanotubes.

    Science.gov (United States)

    Jerez, Javier; Isaguirre, Andrea C; Bazán, Cristian; Martinez, Luis D; Cerutti, Soledad

    2014-06-01

    An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Preconcentration and determination of iron and copper in spice samples by cloud point extraction and flow injection flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sahin, Cigdem Arpa, E-mail: carpa@hacettepe.edu.tr [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey); Tokgoez, Ilknur; Bektas, Sema [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey)

    2010-09-15

    A flow injection (FI) cloud point extraction (CPE) method for the determination of iron and copper by flame atomic absorption spectrometer (FAAS) has been improved. The analytes were complexed with 3-amino-7-dimethylamino-2-methylphenazine (Neutral Red, NR) and octylphenoxypolyethoxyethanol (Triton X-114) was added as a surfactant. The micellar solution was heated above 50 {sup o}C and loaded through a column packed with cotton for phase separation. Then the surfactant-rich phase was eluted using 0.05 mol L{sup -1} H{sub 2}SO{sub 4} and the analytes were determined by FAAS. Chemical and flow variables influencing the instrumental and extraction conditions were optimized. Under optimized conditions for 25 mL of preconcentrated solution, the enrichment factors were 98 and 69, the limits of detection (3s) were 0.7 and 0.3 ng mL{sup -1}, the limits of quantification (10s) were 2.2 and 1.0 ng mL{sup -1} for iron and copper, respectively. The relative standard deviation (RSD) for ten replicate measurements of 10 ng mL{sup -1} iron and copper were 2.1% and 1.8%, respectively. The proposed method was successfully applied to determination of iron and copper in spice samples.

  14. Determination of Noncovalent Binding Using a Continuous Stirred Tank Reactor as a Flow Injection Device Coupled to Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Santos, Inês C.; Waybright, Veronica B.; Fan, Hui; Ramirez, Sabra; Mesquita, Raquel B. R.; Rangel, António O. S. S.; Fryčák, Petr; Schug, Kevin A.

    2015-07-01

    Described is a new method based on the concept of controlled band dispersion, achieved by hyphenating flow injection analysis with ESI-MS for noncovalent binding determinations. A continuous stirred tank reactor (CSTR) was used as a FIA device for exponential dilution of an equimolar host-guest solution over time. The data obtained was treated for the noncovalent binding determination using an equimolar binding model. Dissociation constants between vancomycin and Ac-Lys(Ac)-Ala-Ala-OH peptide stereoisomers were determined using both the positive and negative ionization modes. The results obtained for Ac- L-Lys(Ac)- D-Ala- D-Ala (a model for a Gram-positive bacterial cell wall) binding were in reasonable agreement with literature values made by other mass spectrometry binding determination techniques. Also, the developed method allowed the determination of dissociation constants for vancomycin with Ac- L-Lys(Ac)- D-Ala- L-Ala, Ac- L-Lys(Ac)- L-Ala- D-Ala, and Ac- L-Lys(Ac)- L-Ala- L-Ala. Although some differences in measured binding affinities were noted using different ionization modes, the results of each determination were generally consistent. Differences are likely attributable to the influence of a pseudo-physiological ammonium acetate buffer solution on the formation of positively- and negatively-charged ionic complexes.

  15. Flow injection determination of diclofenac sodium based on its sensitizing effect on the chemiluminescent reaction of acidic potassium permanganate-formaldehyde.

    Science.gov (United States)

    Song, Jingjing; Sun, Pulv; Ji, Zhongling; Li, Jianguo

    2015-02-01

    A sensitive and simple chemiluminescent (CL) method for the determination of diclofenac sodium has been developed by combining the flow injection technique and its sensitizing effect on the weak CL reaction between formaldehyde and acidic potassium permanganate. A calibration curve is constructed for diclofenac sodium under optimized experimental parameters over the range 0.040-5.0 µg/mL and the limit of detection is 0.020 µg/mL (3σ). The inter-assay relative standard deviation for 0.040 µg/mL diclofenac sodium (n = 11) is 2.0%. This method is rapid, sensitive, simple, and shows good selectivity and reproducibility. The proposed method has been successfully applied to the determination of the studied diclofenac sodium in pharmaceutical preparations with satisfactory results. Furthermore, the possible mechanism for the CL reaction has been discussed in detail on the basis of UV and CL spectra. Copyright © 2014 John Wiley & Sons, Ltd.

  16. Potentiometric flow injection system for determination of reductants using a polymeric membrane permanganate ion-selective electrode based on current-controlled reagent delivery.

    Science.gov (United States)

    Song, Wenjing; Ding, Jiawang; Liang, Rongning; Qin, Wei

    2011-10-17

    A polymeric membrane permanganate-selective electrode has been developed as a current-controlled reagent release system for potentiometric detection of reductants in flow injection analysis. By applying an external current, diffusion of permanganate ions across the polymeric membrane can be controlled precisely. The permanganate ions released at the sample-membrane interface from the inner filling solution of the electrode are consumed by reaction with a reductant in the sample solution thus changing the measured membrane potential, by which the reductant can be sensed potentiometrically. Ascorbate, dopamine and norepinephrine have been employed as the model reductants. Under the optimized conditions, the potential peak heights are proportional to the reductant concentrations in the ranges of 1.0×10(-5) to 2.5×10(-7)M for ascorbate, of 1.0×10(-5) to 5.0×10(-7)M for dopamine, and of 1.0×10(-5) to 5.0×10(-7)M for norepinephrine, respectively with the corresponding detection limits of 7.8×10(-8), 1.0×10(-7) and 1.0×10(-7)M. The proposed system has been successfully applied to the determination of reductants in pharmaceutical preparations and vegetables, and the results agree well with those of iodimetric analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. In-line electrochemical reagent generation coupled to a flow injection biamperometric system for the determination of sulfite in beverage samples.

    Science.gov (United States)

    de Paula, Nattany T G; Barbosa, Elaine M O; da Silva, Paulo A B; de Souza, Gustavo C S; Nascimento, Valberes B; Lavorante, André F

    2016-07-15

    This work reports an in-line electrochemical reagent generation coupled to a flow injection biamperometric procedure for the determination of SO3(2-). The method was based on a redox reaction between the I3(-) and SO3(2-) ions, after the diffusion of SO2 through a gas diffusion chamber. Under optimum experimental conditions, a linear response ranging from 1.0 to 12.0 mg L(-1) (R=0.9999 and n=7), a detection and quantification limit estimated at 0.26 and 0.86 mg L(-1), respectively, a standard deviation relative of 0.4% (n=10) for a reference solution of 4.0 mg L(-1) SO3(2-) and sampling throughput for 40 determinations per hour were achieved. Addition and recovery tests with juice and wine samples were performed resulting in a range between 92% and 110%. There were no significant differences at a 95% confidence level in the analysis of eight samples when comparing the new method with a reference procedure. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Development of a reagentless electrochemiluminescent electrode for flow injection analysis using copolymerised luminol/aniline on nano-TiO2 functionalised indium-tin oxide glass.

    Science.gov (United States)

    Liu, Chao; Wei, Xiuhua; Tu, Yifeng

    2013-07-15

    In this study, a nano-structured copolymer of luminol/aniline (PLA) was deposited onto nano-TiO2-functionalised indium tin oxide (ITO)-coated glass by electrochemical polymerisation using cyclic voltammetry (CV). The resulting reagentless electrochemiluminescent (ECL) electrode (ECLode) can be used for flow injection analysis (FIA). The properties of the ECLode were characterised by CV, electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM). The ECLode has high background ECL emission as well as excellent stability and reproducibility, and yielding sensitive response towards target analytes. The ECL emissions of the ECLode were 50 times higher than PLA/ITO, and 500 times higher than polyluminol (PL)/ITO. The ECLode showed sensitive responses to reactive oxygen species (ROSs), permitting its application for determination of antioxidants by quenching. Under optimised conditions, an absolute detection limit of 69.9 pg was obtained for resveratrol, comparable to the highest levels of sensitivity achieved by other methods. Thus, the gross antioxidant content of red wine was determined, with satisfactory recoveries between 87.6% and 108.3%. These results suggest a bright future for the use of the ECLode for single-channel FIA due to its high sensitivity, accuracy and reproducibility. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Investigation of corrosion behavior of biodegradable magnesium alloys using an online-micro-flow capillary flow injection inductively coupled plasma mass spectrometry setup with electrochemical control

    Energy Technology Data Exchange (ETDEWEB)

    Ulrich, A., E-mail: andrea.ulrich@empa.ch [Laboratory for Analytical Chemistry, EMPA, Swiss Federal Laboratories for Materials Science and Technology, Ueberlandstrasse 129, 8600 Duebendorf (Switzerland); Ott, N. [Laboratory for Analytical Chemistry, EMPA, Swiss Federal Laboratories for Materials Science and Technology, Ueberlandstrasse 129, 8600 Duebendorf (Switzerland); EPFL-Ecole Polytechnique Federale de Lausanne, 1015 Lausanne (Switzerland); Tournier-Fillon, A. [Laboratory for Corrosion and Material Integrity, EMPA, Swiss Federal Laboratories for Materials Science and Technology, Ueberlandstrasse 129, 8600 Duebendorf (Switzerland); Homazava, N. [Laboratory for Analytical Chemistry, EMPA, Swiss Federal Laboratories for Materials Science and Technology, Ueberlandstrasse 129, 8600 Duebendorf (Switzerland); Swiss Centre for Applied Ecotoxicology, Eawag/EPFL, Ueberlandstrasse 133, 8600 Duebendorf (Switzerland); Schmutz, P. [Laboratory for Corrosion and Material Integrity, EMPA, Swiss Federal Laboratories for Materials Science and Technology, Ueberlandstrasse 129, 8600 Duebendorf (Switzerland)

    2011-07-15

    The development of biodegradable metallic materials designed for implants or medical stents is new and is one of the most interesting new fields in material science. Besides biocompatibility, a detailed understanding of corrosion mechanisms and dissolution processes is required to develop materials with tailored degradation behavior. The materials need to be sufficiently stable as long as they have to fulfill their medical task. However, subsequently they should dissolve completely in a controlled manner in terms of maximum body burden. This study focuses on the elemental and time resolved dissolution processes of a magnesium rare earth elements alloy which has been compared to pure magnesium with different impurity level. The here described investigations were performed using a novel analytical setup based on a micro-flow capillary online-coupled via a flow injection system to a plasma mass spectrometer. Differences in element-specific and time-dependent dissolution were monitored for various magnesium alloys in contact with sodium chloride or mixtures of sodium and calcium chloride as corrosive media. The dissolution behavior strongly depends on bulk matrix elements, secondary alloying elements and impurities, which are usually present even in pure magnesium.

  20. Investigation of corrosion behavior of biodegradable magnesium alloys using an online-micro-flow capillary flow injection inductively coupled plasma mass spectrometry setup with electrochemical control

    International Nuclear Information System (INIS)

    Ulrich, A.; Ott, N.; Tournier-Fillon, A.; Homazava, N.; Schmutz, P.

    2011-01-01

    The development of biodegradable metallic materials designed for implants or medical stents is new and is one of the most interesting new fields in material science. Besides biocompatibility, a detailed understanding of corrosion mechanisms and dissolution processes is required to develop materials with tailored degradation behavior. The materials need to be sufficiently stable as long as they have to fulfill their medical task. However, subsequently they should dissolve completely in a controlled manner in terms of maximum body burden. This study focuses on the elemental and time resolved dissolution processes of a magnesium rare earth elements alloy which has been compared to pure magnesium with different impurity level. The here described investigations were performed using a novel analytical setup based on a micro-flow capillary online-coupled via a flow injection system to a plasma mass spectrometer. Differences in element-specific and time-dependent dissolution were monitored for various magnesium alloys in contact with sodium chloride or mixtures of sodium and calcium chloride as corrosive media. The dissolution behavior strongly depends on bulk matrix elements, secondary alloying elements and impurities, which are usually present even in pure magnesium.

  1. One-shot flow injection spectrophotometric simultaneous determination of copper, iron and zinc in patients' sera with newly developed multi-compartment flow cell

    International Nuclear Information System (INIS)

    Teshima, Norio; Gotoh, Shingo; Ida, Kazunori; Sakai, Tadao

    2006-01-01

    We propose here an affordable flow injection method for simultaneous spectrophotometric determination of copper, iron and zinc in patients' sera. The use of a newly designed multi-compartment flow cell allowed the simultaneous determination of the three metals with a single injection ('one-shot') and a double beam spectrophotometer. The chemistry relied on the reactions of these metals with 2-(5-nitro-2-pyridylazo)-5-[N-propyl-N-(3-sulfopropyl)amino]phenol (nitro-PAPS) to form corresponding colored complexes. At pH 3.8, only copper-nitro-PAPS complex was formed in the presence of pyrophosphate as a masking agent for iron, and then the copper and iron(II) complexes were formed in the presence of reductant (ascorbic acid) at the same pH, and finally all three metals reacted with nitro-PAPS at pH 8.6. The characteristics were introduced into the flow system to determine each metal selectively and sensitively. Under the optimum conditions, linear calibration curves for the three metals were obtained in the range of 0.01-1 mg L -1 with a sample throughput rate of 20 h -1 . The limits of detection (3σ) were 3.9 μg L -1 for copper, 4.1 μg L -1 for iron and 4.0 μg L -1 for zinc. The proposed method was applied to analysis of some patients' sera

  2. A comparison of continuous pneumatic nebulization and flow injection-direct injection nebulization for sample introduction in inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Crain, J.S.; Kiely, J.T.

    1995-08-01

    Dilute nitric acid blanks and solutions containing Ni, Cd, Pb, and U (including two laboratory waste samples) were analyzed eighteen times over a two-month period using inductively coupled plasma-mass spectrometry (ICP-MS). Two different sample introduction techniques were employed: flow injection-direct injection nebulization (FI-DIN) and continuous pneumatic nebulization (CPN). Using comparable instrumental measurement procedures, FI-DIN analyses were 33% faster and generated 52% less waste than CPN analyses. Instrumental limits of detection obtained with FI-DIN and CPN were comparable but not equivalent (except in the case of Pb) because of nebulizer-related differences in sensitivity (i.e., signal per unit analyte concentration) and background. Substantial and statistically significant differences were found between FI-DIN and CPN Ni determinations, and in the case of the laboratory waste samples, there were also small but statistically significant differences between Cd determinations. These small (2 to 3%) differences were not related to polyatomic ion interference (e.g., 95 Mo 16 O + ), but in light of the time savings and waste reduction to be realized, they should not preclude the use of FI-DIN in place of CPN for determination of Cd, Pb, U and chemically

  3. Preparation of Fe(3)O(4)@C@CNC multifunctional magnetic core/shell nanoparticles and their application in a signal-type flow-injection photoluminescence immunosensor.

    Science.gov (United States)

    Chu, Chengchao; Li, Meng; Li, Long; Ge, Shenguang; Ge, Lei; Yu, Jinghua; Yan, Mei; Song, Xianrang

    2013-11-01

    We describe here the preparation of carbon-coated Fe3O4 magnetic nanoparticles that were further fabricated into multifunctional core/shell nanoparticles (Fe3O4@C@CNCs) through a layer-by-layer self-assembly process of carbon nanocrystals (CNCs). The nanoparticles were applied in a photoluminescence (PL) immunosensor to detect the carcinoembryonic antigen (CEA), and CEA primary antibody was immobilized onto the surface of the nanoparticles. In addition, CEA secondary antibody and glucose oxidase were covalently bonded to silica nanoparticles. After stepwise immunoreactions, the immunoreagent was injected into the PL cell using a flow-injection PL system. When glucose was injected, hydrogen peroxide was obtained because of glucose oxidase catalysis and quenched the PL of the Fe3O4@C@CNC nanoparticles. The here proposed PL immunosensor allowed us to determine CEA concentrations in the 0.005–50 ng·mL-1 concentration range, with a detection limit of 1.8 pg·mL-1.

  4. High-throughput flow injection analysis mass spectroscopy with networked delivery of color-rendered results. 2. Three-dimensional spectral mapping of 96-well combinatorial chemistry racks.

    Science.gov (United States)

    Görlach, E; Richmond, R; Lewis, I

    1998-08-01

    For the last two years, the mass spectroscopy section of the Novartis Pharma Research Core Technology group has analyzed tens of thousands of multiple parallel synthesis samples from the Novartis Pharma Combinatorial Chemistry program, using an in-house developed automated high-throughput flow injection analysis electrospray ionization mass spectroscopy system. The electrospray spectra of these samples reflect the many structures present after the cleavage step from the solid support. The overall success of the sequential synthesis is mirrored in the purity of the expected end product, but the partial success of individual synthesis steps is evident in the impurities in the mass spectrum. However this latter reaction information, which is of considerable utility to the combinatorial chemist, is effectively hidden from view by the very large number of analyzed samples. This information is now revealed at the workbench of the combinatorial chemist by a novel three-dimensional display of each rack's complete mass spectral ion current using the in-house RackViewer Visual Basic application. Colorization of "forbidden loss" and "forbidden gas-adduct" zones, normalization to expected monoisotopic molecular weight, colorization of ionization intensity, and sorting by row or column were used in combination to highlight systematic patterns in the mass spectroscopy data.

  5. Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

    Science.gov (United States)

    Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

    2018-02-01

    A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

  6. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    Science.gov (United States)

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry in water samples

    Directory of Open Access Journals (Sweden)

    Arpa Şahin Ç.

    2013-04-01

    Full Text Available A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME and flow injection flame atomic absorption spectrometric determination (FI-FAAS method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 – 20.0 ng mL–1 and the limit of detection (3s was 0.18 ng mL–1, the limit of quantification (10s was 0.58 ng mL–1. The relative standard deviation (RSD for 10 replicate measurements of 10 ng mL–1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2 and real water samples and satisfactory results were obtained.

  8. Dispersive liquid-liquid microextraction followed by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) determination of 14 lanthanides from ground water

    International Nuclear Information System (INIS)

    Chandrasekaran, K.; Karunasagar, D.; Arunachalam, J.

    2011-01-01

    The aim of the present work was to develop a dispersive liquid-liquid microextraction (DLLME) method for the sensitive determination of REEs at a few parts per billion in groundwater by flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS). In the developed method, methanol (500 μl) and chloroform (200μl) were used as the disperser and extractant respectively. The REEs were complexed with 4-(2-pyridylazo resorcinol) (PAR) at a pH of 7. Acetate ion was added as an auxiliary ligand for neutralization of the charge on the lanthanide-PAR complex. The disperser (MeOH) - extraction solvent (CHCl 3 ) mixture was rapidly injected using a disposable syringe, thereby forming a cloudy solution. The lanthanide-PAR complex was extracted into the fine droplets of the chloroform dispersed in the aqueous phase. The solution was centrifuged and the aqueous layer at the top was discarded. The REEs were back extracted from the chloroform layer with nitric acid for determination by ICPMS. Important parameters for complex formation and extraction, such as volume of extraction/disperser solvent, extraction time, pH and concentration of the chelating agent and the auxiliary ligand are being optimized using ICP-MS. The optimization is being carried out at 5 μg L -1 concentration level of REE in the initial water sample. Preliminary studies have shown an extraction recovery of 80-85% for all the 14 lanthanide elements and these will be presented

  9. Flow-injection chemiluminescence assay for ultra-trace determination of DNA using rhodamine B-Ce(IV)-DNA ternary system in sulfuric acid media

    International Nuclear Information System (INIS)

    Ma Yongjun; Zhou Min; Jin Xiaoyong; Zhang Ziyu; Teng Xiulan; Chen Hui

    2004-01-01

    A novel flow-injection chemiluminescence method for the determination of DNA at ultra-trace level has been established. In 0.8 M sulfuric acid media, the chemiluminescence of the rhodamine B-cerium (IV) or Ce(IV) system is enhanced by DNA, activated previously by imidazole-HCl buffer solution (pH 7.0). The enhanced intensity of chemiluminescence is in proportion to log DNA concentration 1.0x10 -8 to 0.1 μg ml -1 for herring sperm DNA and 2.0x10 -6 to 0.2 μg ml -1 for calf thymus DNA with 3σ detection limits of 8.3x10 -9 μg ml -1 for herring sperm DNA and 3.5x10 -7 μg ml -1 for calf thymus DNA, respectively. The relative standard deviation for 1.0x10 -4 μg ml -1 herring sperm DNA was 0.99% and 2.0x10 -3 μg ml -1 for calf thymus DNA was 1.1% (n=11). Using the optimized system, DNA contents in six synthetic samples has been determined with recoveries of 99.5-109.0%. The possible mechanism has also been studied in this paper

  10. Flow-injection chemiluminescence assay for ultra-trace determination of DNA using rhodamine B-Ce(IV)-DNA ternary system in sulfuric acid media

    Energy Technology Data Exchange (ETDEWEB)

    Ma Yongjun; Zhou Min; Jin Xiaoyong; Zhang Ziyu; Teng Xiulan; Chen Hui

    2004-01-09

    A novel flow-injection chemiluminescence method for the determination of DNA at ultra-trace level has been established. In 0.8 M sulfuric acid media, the chemiluminescence of the rhodamine B-cerium (IV) or Ce(IV) system is enhanced by DNA, activated previously by imidazole-HCl buffer solution (pH 7.0). The enhanced intensity of chemiluminescence is in proportion to log DNA concentration 1.0x10{sup -8} to 0.1 {mu}g ml{sup -1} for herring sperm DNA and 2.0x10{sup -6} to 0.2 {mu}g ml{sup -1} for calf thymus DNA with 3{sigma} detection limits of 8.3x10{sup -9} {mu}g ml{sup -1} for herring sperm DNA and 3.5x10{sup -7} {mu}g ml{sup -1} for calf thymus DNA, respectively. The relative standard deviation for 1.0x10{sup -4} {mu}g ml{sup -1} herring sperm DNA was 0.99% and 2.0x10{sup -3} {mu}g ml{sup -1} for calf thymus DNA was 1.1% (n=11). Using the optimized system, DNA contents in six synthetic samples has been determined with recoveries of 99.5-109.0%. The possible mechanism has also been studied in this paper.

  11. Investigation of corrosion behavior of biodegradable magnesium alloys using an online-micro-flow capillary flow injection inductively coupled plasma mass spectrometry setup with electrochemical control

    Science.gov (United States)

    Ulrich, A.; Ott, N.; Tournier-Fillon, A.; Homazava, N.; Schmutz, P.

    2011-07-01

    The development of biodegradable metallic materials designed for implants or medical stents is new and is one of the most interesting new fields in material science. Besides biocompatibility, a detailed understanding of corrosion mechanisms and dissolution processes is required to develop materials with tailored degradation behavior. The materials need to be sufficiently stable as long as they have to fulfill their medical task. However, subsequently they should dissolve completely in a controlled manner in terms of maximum body burden. This study focuses on the elemental and time resolved dissolution processes of a magnesium rare earth elements alloy which has been compared to pure magnesium with different impurity level. The here described investigations were performed using a novel analytical setup based on a micro-flow capillary online-coupled via a flow injection system to a plasma mass spectrometer. Differences in element-specific and time-dependent dissolution were monitored for various magnesium alloys in contact with sodium chloride or mixtures of sodium and calcium chloride as corrosive media. The dissolution behavior strongly depends on bulk matrix elements, secondary alloying elements and impurities, which are usually present even in pure magnesium.

  12. On-line determination of glucose and lactate concentrations in animal cell culture based on fibre optic detection of oxygen in flow-injection analysis.

    Science.gov (United States)

    Dremel, B A; Li, S Y; Schmid, R D

    1992-01-01

    A flow-injection analysis (FIA) system based on fibre optic detection of oxygen consumption using immobilized glucose oxidase (GOD) and lactate oxidase (LOD) is described for the on-line monitoring of glucose and lactate concentrations in animal cell cultures. The consumption of oxygen was determined via dynamic quenching by molecular oxygen of the fluorescence of an indicator. GOD and LOD were immobilized on controlled pore glass (CPG) in enzyme reactors which were directly linked to a specially designed fibre optic flow-through cell covering the oxygen optrode. The system is linear for 0-30 mM glucose, with an r.s.d. of 5% at 30 mM (five measurements) and for 0-30 mM lactate, with an r.s.d. of 5% at 30 mM (five measurements). The enzyme reactors used were stable for more than 4 weeks in continuous operation, and it was possible to analyse up to 20 samples per hour. The system has been successfully applied to the on-line monitoring of glucose and lactate concentrations of an animal cell culture designed for the production of recombinant human antithrombine III (AT-III). Results of the on-line measurement obtained by the FIA system were compared with the off-line results obtained by a glucose and lactate analyser from Yellow Springs Instrument Company (YSI).

  13. Adaptation of a load-inject valve for a flow injection chemiluminescence system enabling dual-reagent injection enhances understanding of environmental Fenton chemistry

    International Nuclear Information System (INIS)

    Jones, Matthew R.; Nightingale, Philp D.; Turner, Suzanne M.; Liss, Peter S.

    2013-01-01

    Graphical abstract: -- Highlights: •Measurement of multiple components of Fenton chemistry; Fe(II) and H 2 O 2 . •Rapid, quasi-simultaneous analysis enables calculation of environmental kinetics. •Low, nano to pico-molar detection limits with dual analyte analysis. •Able to measure complex matrix samples – organically enriched seawater. •Low cost system with appreciable sensitivity compared to single analyte analysis. -- Abstract: Environmental Fenton chemistry has been poorly constrained within the marine environment at a multi-component level. A simple, unique, reconfiguration of a flow-injection analytical system combined with luminol chemiluminescence allows quasi-simultaneously the measurement, using a single load-inject valve and a single photon multiplier tube, of reduced iron, Fe(II), and hydrogen peroxide. The system enables rapid, every 22 s, measurements with good accuracy at environmentally relevant concentrations, less than 5% relative standard deviations on both a 5 nM Fe(II) standard and a 60 nM hydrogen peroxide standard. Limits of detection were as low as 40 pM Fe(II) and 100 pM hydrogen peroxide. The system showed excellent capability by measuring from within an organic rich seawater the photochemically induced production of Fe(II) and hydrogen peroxide and their subsequent cycling and Fenton like interactions

  14. Vesicle Motion during Sustained Exocytosis in Chromaffin Cells: Numerical Model Based on Amperometric Measurements.

    Directory of Open Access Journals (Sweden)

    Daungruthai Jarukanont

    Full Text Available Chromaffin cells release catecholamines by exocytosis, a process that includes vesicle docking, priming and fusion. Although all these steps have been intensively studied, some aspects of their mechanisms, particularly those regarding vesicle transport to the active sites situated at the membrane, are still unclear. In this work, we show that it is possible to extract information on vesicle motion in Chromaffin cells from the combination of Langevin simulations and amperometric measurements. We developed a numerical model based on Langevin simulations of vesicle motion towards the cell membrane and on the statistical analysis of vesicle arrival times. We also performed amperometric experiments in bovine-adrenal Chromaffin cells under Ba2+ stimulation to capture neurotransmitter releases during sustained exocytosis. In the sustained phase, each amperometric peak can be related to a single release from a new vesicle arriving at the active site. The amperometric signal can then be mapped into a spike-series of release events. We normalized the spike-series resulting from the current peaks using a time-rescaling transformation, thus making signals coming from different cells comparable. We discuss why the obtained spike-series may contain information about the motion of all vesicles leading to release of catecholamines. We show that the release statistics in our experiments considerably deviate from Poisson processes. Moreover, the interspike-time probability is reasonably well described by two-parameter gamma distributions. In order to interpret this result we computed the vesicles' arrival statistics from our Langevin simulations. As expected, assuming purely diffusive vesicle motion we obtain Poisson statistics. However, if we assume that all vesicles are guided toward the membrane by an attractive harmonic potential, simulations also lead to gamma distributions of the interspike-time probability, in remarkably good agreement with experiment. We

  15. Vesicle Motion during Sustained Exocytosis in Chromaffin Cells: Numerical Model Based on Amperometric Measurements.

    Science.gov (United States)

    Jarukanont, Daungruthai; Bonifas Arredondo, Imelda; Femat, Ricardo; Garcia, Martin E

    2015-01-01

    Chromaffin cells release catecholamines by exocytosis, a process that includes vesicle docking, priming and fusion. Although all these steps have been intensively studied, some aspects of their mechanisms, particularly those regarding vesicle transport to the active sites situated at the membrane, are still unclear. In this work, we show that it is possible to extract information on vesicle motion in Chromaffin cells from the combination of Langevin simulations and amperometric measurements. We developed a numerical model based on Langevin simulations of vesicle motion towards the cell membrane and on the statistical analysis of vesicle arrival times. We also performed amperometric experiments in bovine-adrenal Chromaffin cells under Ba2+ stimulation to capture neurotransmitter releases during sustained exocytosis. In the sustained phase, each amperometric peak can be related to a single release from a new vesicle arriving at the active site. The amperometric signal can then be mapped into a spike-series of release events. We normalized the spike-series resulting from the current peaks using a time-rescaling transformation, thus making signals coming from different cells comparable. We discuss why the obtained spike-series may contain information about the motion of all vesicles leading to release of catecholamines. We show that the release statistics in our experiments considerably deviate from Poisson processes. Moreover, the interspike-time probability is reasonably well described by two-parameter gamma distributions. In order to interpret this result we computed the vesicles' arrival statistics from our Langevin simulations. As expected, assuming purely diffusive vesicle motion we obtain Poisson statistics. However, if we assume that all vesicles are guided toward the membrane by an attractive harmonic potential, simulations also lead to gamma distributions of the interspike-time probability, in remarkably good agreement with experiment. We also show that

  16. Comparison between amperometric and true potentiometric end-point detection in the determination of water by the Karl Fischer method.

    Science.gov (United States)

    Cedergren, A

    1974-06-01

    A rapid and sensitive method using true potentiometric end-point detection has been developed and compared with the conventional amperometric method for Karl Fischer determination of water. The effect of the sulphur dioxide concentration on the shape of the titration curve is shown. By using kinetic data it was possible to calculate the course of titrations and make comparisons with those found experimentally. The results prove that the main reaction is the slow step, both in the amperometric and the potentiometric method. Results obtained in the standardization of the Karl Fischer reagent showed that the potentiometric method, including titration to a preselected potential, gave a standard deviation of 0.001(1) mg of water per ml, the amperometric method using extrapolation 0.002(4) mg of water per ml and the amperometric titration to a pre-selected diffusion current 0.004(7) mg of water per ml. Theories and results dealing with dilution effects are presented. The time of analysis was 1-1.5 min for the potentiometric and 4-5 min for the amperometric method using extrapolation.

  17. Determination of thiomersal by flow injection coupled with microwave-assisted photochemical online oxidative decomposition of organic mercury and cold vapor atomic fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Campanella, Beatrice; Onor, Massimo; Mascherpa, Marco Carlo; D’Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici-ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ferrari, Carlo [National Research Council of Italy, C.N.R., Istituto Nazionale di Ottica, INO–UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici-ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2013-12-04

    Graphical abstract: -- Highlights: •Thiomersal was determined on line using FI-MW/UV-CVGAFS. •MW/UV allows a “green” on line oxidation of organic mercury to Hg{sup II}. •Each measure requires less than 5 min with a LOD of 3 ng mL{sup −1} (as mercury). •Hg concentration in commercial ophthalmic solutions ranges between 7.5 and 59.0 μg mL{sup −1}. -- Abstract: We developed a flow injection (FI) method for the determination of thiomersal (sodium ethylmercurithiosalicylate, C{sub 9}H{sub 9}HgNaO{sub 2}S) based on the UV/microwave (MW) photochemical, online oxidation of organic mercury, followed by cold vapor generation atomic fluorescence spectrometry (CVG-AFS) detection. Thiomersal was quantitatively converted in the MW/UV process to Hg(II), with a yield of 97 ± 3%. This reaction was followed by the reduction of Hg(II) to Hg(0) performed in a knotted reaction coil with NaBH{sub 4} solution, and AFS detection in an Ar/H{sub 2} miniaturized flame. The method was linear in the 0.01–2 μg mL{sup −1} range, with a LOD of 0.003 μg mL{sup −1}. This method has been applied to the determination of thiomersal in ophthalmic solutions, with recoveries ranging between 97% and 101%. We found a mercury concentration in commercial ophthalmic solutions ranging between 7.5 and 59.0 μg mL{sup −1}.

  18. Determination of thiomersal by flow injection coupled with microwave-assisted photochemical online oxidative decomposition of organic mercury and cold vapor atomic fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Campanella, Beatrice; Onor, Massimo; Mascherpa, Marco Carlo; D’Ulivo, Alessandro; Ferrari, Carlo; Bramanti, Emilia

    2013-01-01

    Graphical abstract: -- Highlights: •Thiomersal was determined on line using FI-MW/UV-CVGAFS. •MW/UV allows a “green” on line oxidation of organic mercury to Hg II . •Each measure requires less than 5 min with a LOD of 3 ng mL −1 (as mercury). •Hg concentration in commercial ophthalmic solutions ranges between 7.5 and 59.0 μg mL −1 . -- Abstract: We developed a flow injection (FI) method for the determination of thiomersal (sodium ethylmercurithiosalicylate, C 9 H 9 HgNaO 2 S) based on the UV/microwave (MW) photochemical, online oxidation of organic mercury, followed by cold vapor generation atomic fluorescence spectrometry (CVG-AFS) detection. Thiomersal was quantitatively converted in the MW/UV process to Hg(II), with a yield of 97 ± 3%. This reaction was followed by the reduction of Hg(II) to Hg(0) performed in a knotted reaction coil with NaBH 4 solution, and AFS detection in an Ar/H 2 miniaturized flame. The method was linear in the 0.01–2 μg mL −1 range, with a LOD of 0.003 μg mL −1 . This method has been applied to the determination of thiomersal in ophthalmic solutions, with recoveries ranging between 97% and 101%. We found a mercury concentration in commercial ophthalmic solutions ranging between 7.5 and 59.0 μg mL −1

  19. Flow Injection Photochemical Vapor Generation Coupled with Miniaturized Solution-Cathode Glow Discharge Atomic Emission Spectrometry for Determination and Speciation Analysis of Mercury.

    Science.gov (United States)

    Mo, Jiamei; Li, Qing; Guo, Xiaohong; Zhang, Guoxia; Wang, Zheng

    2017-10-03

    A novel, compact, and green method was developed for the determination and speciation analysis of mercury, based on flow injection photochemical vapor generation (PVG) coupled with miniaturized solution cathode glow discharge-atomic emission spectroscopy (SCGD-AES). The SCGD was generated between a miniature hollow titanium tube and a solution emerging from a glass capillary. Cold mercury vapor (Hg(0)) was generated by PVG and subsequently delivered to the SCGD for excitation, and finally the emission signals were recorded by a miniaturized spectrograph. The detection limits (DLs) of Hg(II) and methylmercury (MeHg) were both determined to be 0.2 μg L -1 . Moreover, mercury speciation analysis could also be performed by using different wavelengths and powers from the UV lamp and irradiation times. Both Hg(II) and MeHg can be converted to Hg(0) for the determination of total mercury (T-Hg) with 8 W/254 nm UV lamp and 60 s irradiation time; while only Hg(II) can be reduced to Hg(0) and determined selectively with 4 W/365 nm UV lamp and 20 s irradiation time. Then, the concentration of MeHg can be calculated by subtracting the Hg(II) from the T-Hg. Because of its similar sensitivity and DL at 8 W/254 nm, the simpler and less toxic Hg(II) was used successfully as a primary standard for the quantification of T-Hg. The novel PVG-SCGD-AES system provides not only a 365-fold improvement in the DL for Hg(II) but also a nonchromatographic method for the speciation analysis of mercury. After validating its accuracy, this method was successfully used for mercury speciation analysis of water and biological samples.

  20. Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Department of Chemistry, Xuzhou Normal University, Xuzhou 221116 (China); Jin Yan [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Han Weiying [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Miao, Qiang [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Bi Shuping [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China)]. E-mail: bisp@nju.edu.cn

    2006-07-15

    A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH{sub 4} solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h{sup -1} with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l{sup -1} for Hg{sup 2+} and 2.0 ng l{sup -1} for CH{sub 3}Hg{sup +}. The precisions (RSD) for the 11 replicate measurements of each 0.2 {mu}g l{sup -1} of Hg{sup 2+} and CH{sub 3}Hg{sup +} were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples.

  1. Artificial neural networks study of the catalytic reduction of resazurin: stopped-flow injection kinetic-spectrophotometric determination of Cu(II) and Ni(II)

    International Nuclear Information System (INIS)

    Magni, Diana M.; Olivieri, Alejandro C.; Bonivardi, Adrian L.

    2005-01-01

    An artificial neural network (ANN) procedure was used in the development of a catalytic spectrophotometric method for the determination of Cu(II) and Ni(II) employing a stopped-flow injection system. The method is based on the catalytic action of these ions on the reduction of resazurin by sulfide. ANNs trained by back-propagation of errors allowed us to model the systems in a concentration range of 0.5-6 and 1-15 mg l -1 for Cu(II) and Ni(II), respectively, with a low relative error of prediction (REP) for each cation: REP Cu(II) = 0.85% and REP Ni(II) = 0.79%. The standard deviations of the repeatability (s r ) and of the within-laboratory reproducibility (s w ) were measured using standard solutions of Cu(II) and Ni(II) equal to 2.75 and 3.5 mg l -1 , respectively: s r [Cu(II)] = 0.039 mg l -1 , s r [Ni(II)] = 0.044 mg l -1 , s w [Ni(II)] = 0.045 mg l -1 and s w [Ni(II)] = 0.050 mg l -1 . The ANNs-kinetic method has been applied to the determination of Cu(II) and Ni(II) in electroplating solutions and provided satisfactory results as compared with flame atomic absorption spectrophotometry method. The effect of resazurin, NaOH and Na 2 S concentrations and the reaction temperature on the analytical sensitivity is discussed

  2. Novel PVC-membrane potentiometric sensors based on a recently synthesized sulfur-containing macrocyclic diamide for Cd2+ ion. Application to flow-injection potentiometry.

    Science.gov (United States)

    Shamsipur, Mojtaba; Dezaki, Abbas Shirmardi; Akhond, Morteza; Sharghi, Hashem; Paziraee, Zahra; Alizadeh, Kamal

    2009-12-30

    A new sulfur-containing macrocyclic diamide, 1,15-diaza-3,4,12,13-dibenzo-5,11-dithia-8-oxa-1,15-(2,6-pyrido)cyclooctadecan-2,14-dione, L, was synthesized, characterized and used as an active component for fabrication of PVC-based polymeric membrane (PME), coated graphite (CGE) and coated silver wire electrodes (CWE) for sensing Cd(2+) ion. The electrodes exhibited linear Nernstian responses to Cd(2+) ion in the concentration range of 3.3 x 10(-6) to 3.3 x 10(-1)M (for PME, LOD=1.2 x 10(-6)M), 2.0 x 10(-7) to 3.3 x 10(-1)M (for CWE, LOD=1.3 x 10(-7)M) and 1.6 x 10(-8) to 1.3 x 10(-1)M (for CGE, LOD=1.0 x 10(-8)M). The CGE was used as a proper detection system in flow-injection potentiometry (FIP) with a linear Nernstian range of 3.2 x 10(-8) to 1.4 x 10(-1)M (LOD=1.3 x 10(-8)M). The optimum pH range was 3.5-7.6. The electrodes revealed fairly good discriminating ability towards Cd(2+) in comparison with a large number of alkali, alkaline earth, transition and heavy metal ions. The electrodes found to be chemically inert, showing a fast response time of <5s, and could be used practically over a period of about 2-3 months. The practical utility of the proposed system has also been reported.

  3. Simple and ultra-fast recognition and quantitation of compounded monoclonal antibodies: Application to flow injection analysis combined to UV spectroscopy and matching method.

    Science.gov (United States)

    Jaccoulet, E; Schweitzer-Chaput, A; Toussaint, B; Prognon, P; Caudron, E

    2018-09-01

    Compounding of monoclonal antibody (mAbs) constantly increases in hospital. Quality control (QC) of the compounded mAbs based on quantification and identification is required to prevent potential errors and fast method is needed to manage outpatient chemotherapy administration. A simple and ultra-fast (less than 30 s) method using flow injection analysis associated to least square matching method issued from the analyzer software was performed and evaluated for the routine hospital QC of three compounded mAbs: bevacizumab, infliximab and rituximab. The method was evaluated through qualitative and quantitative parameters. Preliminary analysis of the UV absorption and second derivative spectra of the mAbs allowed us to adapt analytical conditions according to the therapeutic range of the mAbs. In terms of quantitative QC, linearity, accuracy and precision were assessed as specified in ICH guidelines. Very satisfactory recovery was achieved and the RSD (%) of the intermediate precision were less than 1.1%. Qualitative analytical parameters were also evaluated in terms of specificity, sensitivity and global precision through a matrix of confusion. Results showed to be concentration and mAbs dependant and excellent (100%) specificity and sensitivity were reached within specific concentration range. Finally, routine application on "real life" samples (n = 209) from different batch of the three mAbs complied with the specifications of the quality control i.e. excellent identification (100%) and ± 15% of targeting concentration belonging to the calibration range. The successful use of the combination of second derivative spectroscopy and partial least square matching method demonstrated the interest of FIA for the ultra-fast QC of mAbs after compounding using matching method. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. A flow injection analysis system for monitoring silver (I) ion and iodine residuals in recycled water from recovery systems used for spaceflight

    International Nuclear Information System (INIS)

    Williamson, Jill P.; Emmert, Gary L.

    2013-01-01

    Graphical abstract: A device for on-line monitoring of the water disinfectants silver (I) ion or iodine in recycled water is presented. Simply change the reagents and the sample loop volume to switch between silver ion and iodine configurations. -- Highlights: •Automated FIA device for monitoring Ag + or I 2 residuals in recycled drinking water. •Method detection limits of Ag + of 52 μg L −1 and I 2 of 2 μg L −1 . •Mean % recoveries for Ag + of 104 ± 1% and for I 2 of 96.2 ± 0.1%. •% relative standard deviation estimates for Ag + of 1.4% and for I 2 of 5.7%. •Bias measurements agreed to 11.3 μg L −1 for Ag + and to 27.3 μg L −1 for I 2 . -- Abstract: A laboratory-built flow injection analyzer is reported for monitoring the drinking water disinfectants silver (I) ion and iodine in water produced from NASA's water recovery system. This analyzer uses spectrophotometric detection with a custom made 10 cm optical flow cell. Optimization and interference studies are discussed for the silver (I) ion configuration. Subsequent results using the silver (I) configuration with minor modifications and alternative reagents gave promising results for iodine determinations as well. The estimated MDL values for Ag + and I 2 are 52 μg L −1 Ag + and 2 μg L −1 I 2 ; the mean percent recoveries were 104% and 96.2% for Ag + and I 2 respectfully; and percent relative standard deviations were estimated at 1.4% for Ag + and 5.7% for I 2 . The agreement of this potentially multifunctional analyzer to reference methods for each respective water disinfectant is measured using Bland–Altman analysis as well as more traditional estimates

  5. Determination of phenols by flow injection and liquid chromatography with on-line quinine-sensitized photo-oxidation and quenched luminol chemiluminescence detection

    International Nuclear Information System (INIS)

    Zhang Wei; Danielson, Neil D.

    2003-01-01

    An on-line quinine-sensitized photo-oxidation with quenched chemiluminescence (CL) detection method is developed for phenols using flow injection (FI) and liquid chromatography (LC). This detection method is based on the decrease of light emission from the luminol CL reaction due to the photo-oxidation of phenols that scavenge the photogenerated reactive oxygen species (e.g. singlet oxygen ( 1 O 2 ) and superoxide (O 2 · - )). On-line photo-oxidation is achieved using a coil photo-reactor made from fluoroethylene-propylene copolymer tubing (3048 mmx0.25 mm i.d.) coiled around a mercury UV lamp. A buffer of pH 7 and a concentration of 350 μM for quinine sulfate are determined optimum for the sensitized photo-oxidation. Using a carrier system flow rate of 60 μl/min, calibration curves taken by FI for 10 phenolic compounds in aqueous solutions showed this decreasing sensitivity order: 4-chlorophenol, phenol, 4-nitrophenol, 3-hydroxy-L-kynurenine, 2-nitrophenol, salicylate, 3-nitrophenol, catechol, 2,4-dinitrophenol, and 2,4-dichlorophenol. This detection method using two tandem coil photo-reactors is also applied for the LC separation of phenol, 4-nitrophenol and 4-chlorophenol on an octadecyl (C18) silica LC column using acetonitrile-H 2 O (40:60, v/v) as a mobile phase. The quenched CL detection limits (about 1 μM or 20 pmol) for phenol and 4-chlorophenol are comparable to those for UV detection at 254 nm. Some selectivity in the quenched CL detection is evident by no interference in the FI phenol response even when benzaldehyde and phenethanol concentrations are 8 and 15 times that of phenol

  6. Determination of arsenic species in human urine using HPLC with on-line photooxidation or microwave-assisted oxidation combined with flow-injection HG-AAS

    Energy Technology Data Exchange (ETDEWEB)

    Sur, R.; Begerow, J.; Dunemann, L. [Department of Analytical Chemistry, Medizinisches Institut fuer Umwelthygiene, Duesseldorf (Germany)

    1999-03-01

    An improved analytical procedure is presented for the separation and simultaneous determination of hydride-forming (toxic) and not hydride-forming (non-toxic) arsenic species in human urine. Separation was performed by cation-exchange chromatography using a new solid phase type based on the continuous bed chromatography (CBC) technology. This column permits by a factor of 4 higher flow rates than conventional columns resulting in a drastical reduction of retention times without any loss of resolution. Using this type of column, arsenobetaine (AsBet), arsenocholine (AsChol), and dimethylarsinic acid (DMA) were separated from the more toxic arsenic species arsenous acid (As(III)), arsenic acid (As(V)), and methylarsonic acid (MA) within only 4 min. The HPLC system was coupled via a flow injection system and either a UV or a microwave (MW) reactor to the HG-AAS instrument. UV photolysis and MW digestion were used to transform AsBet and AsChol to hydride-forming species and to make them accessible to HG-AAS. UV photolysis turned out to be more suitable for this application than MW digestion, because the latter technique led to peak broadening and poorer performance. The described procedure was applied to the determination of arsenic species in urine samples of non-occupationally exposed persons before and 12 h after seafood consumption. Detection limits were about 1 {mu}g/L for each arsenic species. After consumption, the AsBet and DMA excretion increased by at least a factor of 150 for AsBet and by a factor of 6 for DMA, respectively, while the excretion of the other species did not increase significantly. This invalidates the use of total urinary arsenic as well as total hydride-forming arsenic as an indicator for exposure to inorganic arsenic. (orig.) With 4 figs., 2 tabs., 13 refs.

  7. Slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry for the determination of trace Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wei-Ni [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Jiang, Shiuh-Jen, E-mail: sjjiang@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Chen, Yen-Ling [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Sahayam, A.C. [National Centre for Compositional Characterisation of Materials (CCCM), Hyderabad (India)

    2015-02-20

    Highlights: • Determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions in a single run. • Accurate analysis using isotope dilution and standard addition methods. • Vapor generation ICP-MS yielded superior detection limits compared to ETV-ICP-MS. • No sample dissolution increased sample through put. • Analysis of GBW09305 Cosmetic (Cream) reference material for accuracy. - Abstract: A slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) method has been developed for the determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions using flow injection (FI) vapor generation (VG) as the sample introduction system. A slurry containing 2% m/v lotion, 2% m/v thiourea, 0.05% m/v L-cysteine, 0.5 μg mL{sup −1} Co(II), 0.1% m/v Triton X-100 and 1.2% v/v HCl was injected into a VG-ICP-MS system for the determination of Ge, As, Cd, Sb, Hg and Bi without dissolution and mineralization. Because the sensitivities of the analytes in the slurry and that of aqueous solution were quite different, an isotope dilution method and a standard addition method were used for the determination. This method has been validated by the determination of Ge, As, Cd, Sb, Hg and Bi in GBW09305 Cosmetic (Cream) reference material. The method was also applied for the determination of Ge, As, Cd, Sb, Hg and Bi in three cosmetic lotion samples obtained locally. The analysis results of the reference material agreed with the certified value and/or ETV-ICP-MS results. The detection limit estimated from the standard addition curve was 0.025, 0.1, 0.2, 0.1, 0.15, and 0.03 ng g{sup −1} for Ge, As, Cd, Sb, Hg and Bi, respectively, in original cosmetic lotion sample.

  8. Slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry for the determination of trace Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions

    International Nuclear Information System (INIS)

    Chen, Wei-Ni; Jiang, Shiuh-Jen; Chen, Yen-Ling; Sahayam, A.C.

    2015-01-01

    Highlights: • Determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions in a single run. • Accurate analysis using isotope dilution and standard addition methods. • Vapor generation ICP-MS yielded superior detection limits compared to ETV-ICP-MS. • No sample dissolution increased sample through put. • Analysis of GBW09305 Cosmetic (Cream) reference material for accuracy. - Abstract: A slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) method has been developed for the determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions using flow injection (FI) vapor generation (VG) as the sample introduction system. A slurry containing 2% m/v lotion, 2% m/v thiourea, 0.05% m/v L-cysteine, 0.5 μg mL −1 Co(II), 0.1% m/v Triton X-100 and 1.2% v/v HCl was injected into a VG-ICP-MS system for the determination of Ge, As, Cd, Sb, Hg and Bi without dissolution and mineralization. Because the sensitivities of the analytes in the slurry and that of aqueous solution were quite different, an isotope dilution method and a standard addition method were used for the determination. This method has been validated by the determination of Ge, As, Cd, Sb, Hg and Bi in GBW09305 Cosmetic (Cream) reference material. The method was also applied for the determination of Ge, As, Cd, Sb, Hg and Bi in three cosmetic lotion samples obtained locally. The analysis results of the reference material agreed with the certified value and/or ETV-ICP-MS results. The detection limit estimated from the standard addition curve was 0.025, 0.1, 0.2, 0.1, 0.15, and 0.03 ng g −1 for Ge, As, Cd, Sb, Hg and Bi, respectively, in original cosmetic lotion sample

  9. On-line complexation/cloud point preconcentration for the sensitive determination of dysprosium in urine by flow injection inductively coupled plasma-optical emission spectrometry

    International Nuclear Information System (INIS)

    Ortega, Claudia; Cerutti, Soledad; Silva, Maria F.; Olsina, Roberto A.; Martinez, Luis D.

    2003-01-01

    An on-line dysprosium preconcentration and determination system based on the hyphenation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with ICP-OES was studied. For the preconcentration of dysprosium, a Dy(III)-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex was formed on-line at pH 9.22 in the presence of nonionic micelles of PONPE-7.5. The micellar system containing the complex was thermostated at 30 C in order to promote phase separation, and the surfactant-rich phase was retained in a microcolumn packed with cotton at pH 9.2. The surfactant-rich phase was eluted with 4 mol L -1 nitric acid at a flow rate of 1.5 mL min -1 , directly in the nebulizer of the plasma. An enhancement factor of 50 was obtained for the preconcentration of 50 mL of sample solution. The detection limit value for the preconcentration of 50 mL of aqueous solution of Dy was 0.03 μg L -1 . The precision for 10 replicate determinations at the 2.0 μg L -1 Dy level was 2.2% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for dysprosium was linear with a correlation coefficient of 0.9994 at levels near the detection limits up to at least 100 μg L -1 . The method was successfully applied to the determination of dysprosium in urine. (orig.)

  10. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sahin, Cigdem Arpa; Tokgoez, Ilknur

    2010-01-01

    A rapid, simple and cost effective solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper was developed. In this method, a free microdrop of 1-undecanol containing 1,5-diphenyl carbazide (DPC) as the complexing agent was transferred to the surface of an aqueous sample including Cu(II) ions, while being agitated by a stirring bar in the bulk of the solution. Under the proper stirring conditions, the suspended microdrop can remain at the top-center position of the aqueous sample. After the completion of the extraction, the sample vial was cooled by placing it in a refrigerator for 10 min. The solidified microdrop was then transferred into a conical vial, where it melted immediately and diluted to 300 μL with ethanol. Finally, copper ions in 200 μL of diluted solution were determined by FI-FAAS. Several factors affecting the microextraction efficiency, such as type of extraction solvent, pH, complexing agent concentration, extraction time, stirring rate, sample volume and temperature were investigated and optimized. Under optimized conditions for 100 mL of solution, the preconcentration factor was 333 and the enrichment factor was 324. The limit of detection (3 s) was 0.4 ng mL -1 , the limit of quantification (10 s) was 1.1 ng mL -1 and the relative standard deviation (RSD) for 10 replicate measurements of 10 ng mL -1 copper was 0.9%. The proposed method was successfully applied to the determination of copper in different water samples.

  11. Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Wu Hong; Jin Yan; Han Weiying; Miao, Qiang; Bi Shuping

    2006-01-01

    A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH 4 solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h -1 with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l -1 for Hg 2+ and 2.0 ng l -1 for CH 3 Hg + . The precisions (RSD) for the 11 replicate measurements of each 0.2 μg l -1 of Hg 2+ and CH 3 Hg + were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples

  12. Separation and determination of alditols and sugars by high-pH anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Andersen, Rikke; Sørensen, A.

    2000-01-01

    Carbohydrates such as alditols (polyols or sugar alcohols), monosaccharides and disaccharides are separated as anions by anion-exchange chromatography with a sodium hydroxide eluent, MA1 CarboPac column and pulsed amperometric detection. We report a high-pH anion-exchange chromatographic-pulsed a......Carbohydrates such as alditols (polyols or sugar alcohols), monosaccharides and disaccharides are separated as anions by anion-exchange chromatography with a sodium hydroxide eluent, MA1 CarboPac column and pulsed amperometric detection. We report a high-pH anion-exchange chromatographic......-pulsed amperometric detection (HPAEC-PAD) method that determines all the polyols used as food additives in food products and the most commonly found mono- and disaccharides on a routine basis. The linearity, repeatability, internal reproducibility and accuracy are described. The applicability of the method has been...

  13. Alginate copper oxide nano-biocomposite as a novel material for amperometric glucose biosensing

    International Nuclear Information System (INIS)

    Buk, Vuslat; Emregul, Emel; Emregul, Kaan Cebesoy

    2017-01-01

    A novel amperometric glucose biosensor based on alginate-CuO nano-biocomposite and glucose oxidase (GOD) film was developed and characterized. The properties of the alginate-CuO-GOD film were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Amperometric measurements were employed to characterize the analytical performance of the biosensor. Several parameters including amount of alginate, concentration of GOD and cross-linkers, amount of CuO nanoparticles, and effect of pH were studied and optimized. Under optimal conditions, the developed alginate-CuO-GOD biosensor was shown to have two linear ranges; from 0.04 mM to 3 mM (with a correlation coefficient of 0.9996 and the sensitivity of 30.443 μA mM −1 cm −2 ) and from 4 mM to 35 mM (with a correlation coefficient of 0.9994 and the sensitivity of 7.205 μA mM −1 cm −2 ). The overall detection limit was estimated to be 1.6 μM (signal-to-noise ratio of 3) and the K m value of 2.82 mM. The biosensor exhibited rather good performance with long-term stability (remainder of activity is 78% after 15 days) and significant specificity for glucose when compared to possible interfering molecules such as ascorbic acid, uric acid and acetaminophen. - Highlights: • An amperometric biosensor was constructed by using Alginate-CuO nano-biocomposite complexed with Glucose Oxidase • Glucose Oxidase immobilized to the surface via cross-linking. • Alginate-CuO film was characterized by SEM and FTIR. • The biosensor exhibits excellent analytical performance to glucose with a wide linear range and high sensitivity.

  14. Alginate copper oxide nano-biocomposite as a novel material for amperometric glucose biosensing

    Energy Technology Data Exchange (ETDEWEB)

    Buk, Vuslat [Ankara University, Department of Chemistry, Science Faculty, Tandoğan, Ankara 06100 (Turkey); Tyndall National Institute, University College Cork, Dyke Parade, Cork (Ireland); Emregul, Emel, E-mail: eemregul@yahoo.com [Ankara University, Department of Chemistry, Science Faculty, Tandoğan, Ankara 06100 (Turkey); Emregul, Kaan Cebesoy [Ankara University, Department of Chemistry, Science Faculty, Tandoğan, Ankara 06100 (Turkey)

    2017-05-01

    A novel amperometric glucose biosensor based on alginate-CuO nano-biocomposite and glucose oxidase (GOD) film was developed and characterized. The properties of the alginate-CuO-GOD film were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Amperometric measurements were employed to characterize the analytical performance of the biosensor. Several parameters including amount of alginate, concentration of GOD and cross-linkers, amount of CuO nanoparticles, and effect of pH were studied and optimized. Under optimal conditions, the developed alginate-CuO-GOD biosensor was shown to have two linear ranges; from 0.04 mM to 3 mM (with a correlation coefficient of 0.9996 and the sensitivity of 30.443 μA mM{sup −1} cm{sup −2}) and from 4 mM to 35 mM (with a correlation coefficient of 0.9994 and the sensitivity of 7.205 μA mM{sup −1} cm{sup −2}). The overall detection limit was estimated to be 1.6 μM (signal-to-noise ratio of 3) and the K{sub m} value of 2.82 mM. The biosensor exhibited rather good performance with long-term stability (remainder of activity is 78% after 15 days) and significant specificity for glucose when compared to possible interfering molecules such as ascorbic acid, uric acid and acetaminophen. - Highlights: • An amperometric biosensor was constructed by using Alginate-CuO nano-biocomposite complexed with Glucose Oxidase • Glucose Oxidase immobilized to the surface via cross-linking. • Alginate-CuO film was characterized by SEM and FTIR. • The biosensor exhibits excellent analytical performance to glucose with a wide linear range and high sensitivity.

  15. Signal enhancement in amperometric peroxide detection by using graphene materials with low number of defects

    International Nuclear Information System (INIS)

    Zöpfl, Alexander; Matysik, Frank-Michael; Hirsch, Thomas; Sisakthi, Masoumeh; Eroms, Jonathan; Strunk, Christoph

    2016-01-01

    Two-dimensional carbon nanomaterials ranging from single-layer graphene to defective structures such as chemically reduced graphene oxide were studied with respect to their use in electrodes and sensors. Their electrochemical properties and utility in terms of fabrication of sensing devices are compared. Specifically, the electrodes have been applied to reductive amperometric determination of hydrogen peroxide. Low-defect graphene (SG) was obtained through mechanical exfoliation of natural graphite, while higher-defect graphenes were produced by chemical vapor deposition (CVDG) and by chemical oxidation of graphite and subsequent reduction (rGO). The carbonaceous materials were mainly characterized by Raman microscopy. They were applied as electrode material and the electrochemical behavior was investigated by chronocoulometry, cyclic voltammetry, electrochemical impedance spectroscopy and amperometry and compared to a carbon disc electrode. It is shown that the quality of the graphene has an enormous impact on the amperometric performance. The use of carbon materials with many defects (like rGO) does not result in a significant improvement in signal compared to a plain carbon disc electrode. The sensitivity is 173 mA · M −1  · cm −2 in case of using CVDG which is about 50 times better than that of a plain carbon disc electrode and about 7 times better than that of rGO. The limit of detection for hydrogen peroxide is 15.1 μM (at a working potential of −0.3 V vs SCE) for CVDG. It is concluded that the application of two-dimensional carbon nanomaterials offers large perspectives in amperometric detection systems due to electrocatalytic effects that result in highly sensitive detection. (author)

  16. Amperometric titration of thorium and some lanthanoids in acetic-acid medium using two indicator electrodes

    International Nuclear Information System (INIS)

    Khadeev, V.A.; Gevorgyan, A.M.; Talipov, Sh.T.; Kostylev, V.S.

    1979-01-01

    The votammetric behaviour of nitriletrimethylphosphonic acid (NTMP) in the medium of anhydrous acetic acid with different backgrounds in the anode region of polarization of a platinum microdisk electrode, is studied. The optimal conditions are found for the amperometric titration with two indicator electrodes of thorium and same lanthanides by a NTMP solution in anhydrous acetic medium. The influence of foreign anions and cations on the results of titration by the NTPM solution in anhydrous acetic acid is studied. The selectivity of titration in anhydrous medium is higher than in aqueous

  17. Creation of a Databank for Content of Antioxidants in Food Products by an Amperometric Method

    Directory of Open Access Journals (Sweden)

    Polina A. Fedina

    2010-10-01

    Full Text Available Oxidative stress, i.e. excessive content of reactionary, oxygen, and nitrogen compounds (ROAC, including free radicals, is one of the causes of various dangerous diseases as well as premature aging. The adverse effect of free radicals can be neutralized by antioxidants. In order to carry out antioxidant therapy, one needs to know the contents of antioxidants in food products. We have created the databank for the contents of antioxidants in 1,140 food products, beverages, etc. Apart from water-soluble antioxidants, fat-soluble antioxidants in dairy and fish products, cacao, chocolate, nuts etc. were determined for the first time using an amperometric method.

  18. [Study on Content Determination of Lead and Arsenic in Four Traditional Tibetan Medicine Prescription Preparations by Wet Digestion Flow Injection-Hydride Generation-Atomic Absorption Spectrometry].

    Science.gov (United States)

    Zheng, Zhi-yuan; Du, Yu-zhi; Zhang, Ming; Yu, Ming-jie; Li, Cen; Yang, Hong-xia; Zhao, Jing; Xia, Zheng-hua; Wei, Li-xin

    2015-04-01

    Four common traditional tibetan medicine prescription preparations "Anzhijinghuasan, Dangzuo, Renqingchangjue and Rannasangpei" in tibetan areas were selected as study objects in the present study. The purpose was to try to establish a kind of wet digestion and flow injection-hydride generation-atomic absorption spectrometry (FI-HAAS) associated analysis method for the content determinations of lead and arsenic in traditional tibetan medicine under optimized digestion and measurement conditions and determine their contents accurately. Under these optimum operating conditions, experimental results were as follows. The detection limits for lead and arsenic were 0.067 and 0.012 µg · mL(-1) respectively. The quantification limits for lead and arsenic were 0.22 and 0.041 µg · mL(-1) respectively. The linear ranges for lead and arsenic were 25-1,600 ng · mL(-1) (r = 0.9995) and 12.5-800 ng · mL(-1) (r = 0.9994) respectively. The degrees of precision(RSD) for lead and arsenic were 2.0% and 3.2% respectively. The recovery rates for lead and arsenic were 98.00%-99.98% and 96.67%-99.87% respectively. The content determination results of lead and arsenic in four traditional tibetan medicine prescription preparations were as fol- lows. The contents of lead and arsenic in Anzhijinghuasan are 0.63-0.67 µg · g(-1) and 0.32-0.33 µg · g(-1) in Anzhijinghua- san, 42.92-43.36 µg · g(-1) and 24.67-25.87 µg · g(-1) in Dangzuo, 1,611. 39-1,631.36 µg · g(-1) and 926.76-956.52 µg- g(-1) in Renqing Changjue, and 1,102.28-1,119.127 µg-g(-1) and 509.96-516.87 µg · g(-1) in Rannasangpei, respectively. This study established a method for content determination of lead and arsenic in traditional tibetan medicine, and determined the content levels of lead and arsenic in four tibetan medicine-prescription preparations accurately. In addition, these results also provide the basis for the safe and effective use of those medicines in clinic.

  19. Simultaneous quantification of the organophosphorus pesticides dimethoate and omethoate in porcine plasma and urine by LC-ESI-MS/MS and flow-injection-ESI-MS/MS.

    Science.gov (United States)

    John, Harald; Eddleston, Michael; Clutton, R Eddie; Worek, Franz; Thiermann, Horst

    2010-05-15

    Dimethoate is an organophosphorus toxicant used in agri- and horticulture as a systemic broad-spectrum insecticide. It also exhibits toxic activity towards mammalian organism provoked by catalytic desulfuration in the liver producing its oxon-derivative omethoate thus inhibiting acetylcholinesterase, initiating cholinergic crisis and ultimately leading to death by respiratory paralysis and cardiovascular collapse. Pharmaco- and toxicokinetic studies in animal models help to broaden basic understanding of medical intervention by antidotes and supportive care. Therefore, we developed and validated a LC-ESI-MS/MS method suitable for the simultaneous, selective, precise (RSD(intra-day) 1-8%; RSD(inter-day) 5-14%), accurate (intra-day: 95-107%; inter-day: 90-115%), and robust quantification of both pesticides from porcine urine and plasma after deproteinization by precipitation and extensive dilution (1:11,250 for plasma and 1:40,000 for urine). Accordingly, lower limits of quantification (0.24-0.49 microg/ml plasma and 0.78-1.56 microg/ml urine) and lower limits of detection (0.12-0.24 microg/ml plasma and 0.39-0.78 microg/ml urine) were equivalent to quite low absolute on-column amounts (1.1-2.1 pg for plasma and 2.0-3.9 pg for urine). The calibration range (0.24-250 microg/ml plasma and 0.78-200 microg/ml urine) was subdivided into two linear ranges (r(2)>or=0.998) each covering nearly two orders of magnitude. The lack of any interfering peak in 6 individual blank specimens from plasma and urine demonstrated the high selectivity of the method. Furthermore, extensive sample dilution causing lowest concentration of potentially interfering matrix ingredients prompted us to develop and validate an additional flow-injection method (FI-ESI-MS/MS). Validation characteristics were as good as for the chromatographic method but sample throughput was enhanced by a factor of 6. Effects on ionization provoked by plasma and urine matrix from 6 individuals as well as in the

  20. A flow injection analyser conductometric coupled system for the field analysis of free dissolved CO{sub 2} and total dissolved inorganic carbon in natural waters

    Energy Technology Data Exchange (ETDEWEB)

    Martinotti, Valter; Balordi, Marcella; Ciceri, Giovanni [RSE SpA - Environment and Sustainable Development Department, Milan (Italy)

    2012-05-15

    A flow injection analyser coupled with a gas diffusion membrane and a conductometric microdetector was adapted for the field analysis of natural concentrations of free dissolved CO{sub 2} and dissolved inorganic carbon in natural waters and used in a number of field campaigns for marine water monitoring. The dissolved gaseous CO{sub 2} presents naturally, or that generated by acidification of the sample, is separated by diffusion using a hydrophobic semipermeable gas porous membrane, and the permeating gas is incorporated into a stream of deionised water and measured by means of an electrical conductometric microdetector. In order to make the system suitable and easy to use for in-field measurements aboard oceanographic ships, the single components of the analyser were compacted into a robust and easy to use system. The calibration of the system is carried out by using standard solutions of potassium bicarbonate at two concentration ranges. Calibration and sample measurements are carried out inside a temperature-constant chamber at 25 C and in an inert atmosphere (N{sub 2}). The detection and quantification limits of the method, evaluated as 3 and 10 times the standard deviation of a series of measurements of the matrix solution were 2.9 and 9.6 {mu}mol/kg of CO{sub 2}, respectively. Data quality for dissolved inorganic carbon was checked with replicate measurements of a certified reference material (A. Dickson, Scripps Institution of Oceanography, University of California, San Diego), both accuracy and repeatability were -3.3% and 10%, respectively. Optimization, performance qualification of the system and its application in various natural water samples are reported and discussed. In the future, the calibration step will be operated automatically in order to improve the analytical performance and the applicability will be increased in the course of experimental surveys carried out both in marine and freshwater ecosystems. Considering the present stage of

  1. Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry.

    Science.gov (United States)

    Nanita, Sergio C; Padivitage, Nilusha L T

    2013-03-20

    A sample extraction and purification procedure that uses ammonium-salt-induced acetonitrile/water phase separation was developed and demonstrated to be compatible with the recently reported method for pesticide residue analysis based on fast extraction and dilution flow injection mass spectrometry (FED-FI-MS). The ammonium salts evaluated were chloride, acetate, formate, carbonate, and sulfate. A mixture of NaCl and MgSO4, salts used in the well-known QuEChERS method, was also tested for comparison. With thermal decomposition/evaporation temperature of salts resulted in negligible ion source residual under typical electrospray conditions, leading to consistent method performance and less instrument cleaning. Although all ammonium salts tested induced acetonitrile/water phase separation, NH4Cl yielded the best performance, thus it was the preferred salting out agent. The NH4Cl salting out method was successfully coupled with FI/MS/MS and tested for fourteen pesticide active ingredients: chlorantraniliprole, cyantraniliprole, chlorimuron ethyl, oxamyl, methomyl, sulfometuron methyl, chlorsulfuron, triflusulfuron methyl, azimsulfuron, flupyrsulfuron methyl, aminocyclopyrachlor, aminocyclopyrachlor methyl, diuron and hexazinone. A validation study was conducted with nine complex matrices: sorghum, rice, grapefruit, canola, milk, eggs, beef, urine and blood plasma. The method is applicable to all analytes, except aminocyclopyrachlor. The method was deemed appropriate for quantitative analysis in 114 out of 126 analyte/matrix cases tested (applicability rate=0.90). The NH4Cl salting out extraction/cleanup allowed expansion of FI/MS/MS for analysis in food of plant and animal origin, and body fluids with increased ruggedness and sensitivity, while maintaining high-throughput (run time=30s/sample). Limits of quantitation (LOQs) of 0.01mgkg(-1) (ppm), the 'well-accepted standard' in pesticide residue analysis, were achieved in >80% of cases tested; while limits of detection

  2. Flow-through solid-phase based optical sensor for the multisyringe flow injection trace determination of orthophosphate in waters with chemiluminescence detection

    International Nuclear Information System (INIS)

    Morais, Ines P.A.; Miro, Manuel; Manera, Matias; Estela, Jose Manuel; Cerda, Victor; Souto, M. Renata S.; Rangel, Antonio O.S.S.

    2004-01-01

    In this work, a novel flow-through solid-phase based chemiluminescence (CL) optical sensor is described for the trace determination of orthophosphate in waters exploiting the multisyringe flow injection analysis (MSFIA) concept with multicommutation. The proposed time-based injection flow system relies upon the in-line derivatisation of the analyte with ammonium molybdate in the presence of vanadate, and the transient immobilisation of the resulting heteropolyacid in a N-vinylpyrrolidone/divinylbenzene copolymer packed spiral shape flow-through cell located in front of the window of a photomultiplier tube. The simultaneous injection of well-defined slugs of luminol in alkaline medium and methanol solution towards the packed reactor is afterwards performed by proper switching of the solenoid valves. Then, the light emission from the luminol oxidation by the oxidant species retained onto the sorbent material is readily detected. At the same time, the generated molybdenum-blue compound is eluted by the minute amount of injected methanol, rendering the system prepared for a new measuring cycle. Therefore, the devised sensor enables the integration of the solid-phase CL reaction with elution and detection of the emitted light without the typical drawbacks of the molybdenum-blue based spectrophotometric procedures regarding the excess of molybdate anion, which causes high background signals due to its self-reduction. The noteworthy features of the developed CL-MSFIA system are the feasibility to accommodate reactions with different pH requirements and the ability to determine trace levels of orthophosphate in high silicate content samples (Si/P ratios up to 500). Under the optimised conditions, a dynamic linear range from 5 to 50 μg P l -1 for a 1.8 ml sample, repeatability better than 3.0% and a quantification limit of 4 μg P l -1 were attained. The flowing stream system handles 11 analysis h -1 and has been successfully applied to the determination of trace levels of

  3. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sigrist, Mirna, E-mail: msigrist@fiq.unl.edu.ar [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Albertengo, Antonela; Beldomenico, Horacio [Laboratorio Central, Facultad de Ingenieria Quimica, Universidad Nacional del Litoral, Santiago del Estero 2654-Piso 6, (3000) Santa Fe (Argentina); Tudino, Mabel [Laboratorio de Analisis de Trazas, Departamento de Quimica Inorganica, Analitica y Quimica Fisica/INQUIMAE, Facultad de Ciencias Exactas y Naturales, Pabellon II, Ciudad Universitaria (1428), Buenos Aires (Argentina)

    2011-04-15

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH{sub 3} generation using 3.5 mol L{sup -1} HCl as carrier solution and 0.35% (m/v) NaBH{sub 4} in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl{sup -}, SO{sub 4}{sup 2-}, NO{sub 3}{sup -}, HPO{sub 4}{sup 2-}, HCO{sub 3}{sup -} on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C{sub 6}H{sub 8}O{sub 6} solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 {mu}g L{sup -1} and 0.6 {mu}g L{sup -1} for As(III) and inorganic total As, respectively, were obtained for a 500 {mu}L sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h{sup -1}. The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species

  4. A flow injection analysis system for monitoring silver (I) ion and iodine residuals in recycled water from recovery systems used for spaceflight

    Energy Technology Data Exchange (ETDEWEB)

    Williamson, Jill P.; Emmert, Gary L., E-mail: gemmert@memphis.edu

    2013-08-20

    Graphical abstract: A device for on-line monitoring of the water disinfectants silver (I) ion or iodine in recycled water is presented. Simply change the reagents and the sample loop volume to switch between silver ion and iodine configurations. -- Highlights: •Automated FIA device for monitoring Ag{sup +} or I{sub 2} residuals in recycled drinking water. •Method detection limits of Ag{sup +} of 52 μg L{sup −1} and I{sub 2} of 2 μg L{sup −1}. •Mean % recoveries for Ag{sup +} of 104 ± 1% and for I{sub 2} of 96.2 ± 0.1%. •% relative standard deviation estimates for Ag{sup +} of 1.4% and for I{sub 2} of 5.7%. •Bias measurements agreed to 11.3 μg L{sup −1} for Ag{sup +} and to 27.3 μg L{sup −1} for I{sub 2}. -- Abstract: A laboratory-built flow injection analyzer is reported for monitoring the drinking water disinfectants silver (I) ion and iodine in water produced from NASA's water recovery system. This analyzer uses spectrophotometric detection with a custom made 10 cm optical flow cell. Optimization and interference studies are discussed for the silver (I) ion configuration. Subsequent results using the silver (I) configuration with minor modifications and alternative reagents gave promising results for iodine determinations as well. The estimated MDL values for Ag{sup +} and I{sub 2} are 52 μg L{sup −1} Ag{sup +} and 2 μg L{sup −1} I{sub 2}; the mean percent recoveries were 104% and 96.2% for Ag{sup +} and I{sub 2} respectfully; and percent relative standard deviations were estimated at 1.4% for Ag{sup +} and 5.7% for I{sub 2}. The agreement of this potentially multifunctional analyzer to reference methods for each respective water disinfectant is measured using Bland–Altman analysis as well as more traditional estimates.

  5. Ion Imprinted Polymer for Preconcentration and Determination of Ultra-Trace Cadmium, Employing Flow Injection Analysis with Thermo Spray Flame Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    do Lago, Ayla Campos; Marchioni, Camila; Mendes, Tássia Venga; Wisniewski, Célio; Fadini, Pedro Sergio; Luccas, Pedro Orival

    2016-11-01

    This work proposes a preconcentration method using an ion imprinted polymer (IIP) for determination of cadmium, in several samples, employing a mini-column filled with the polymer coupled into a flow injection analysis system with detection by thermospray flame furnace atomic absorption spectrometry (FIA-TS-FF-AAS). The polymer was synthesized via bulk using methacrylic acid and vinylimidazole as a functional monomer. For the FIA system initial assessment, the variables: pH, eluent concentration and buffer concentration were studied, employing a 23 full factorial design. To obtain the optimum values for each significant variable, a Doehlert matrix was employed. After the optimization conditions as: pH 5.8, eluent (HNO3) concentration of 0.48 mol L -1 and buffer concentration of 0.01 mol L -1 , were adopted. The proposed method showed a linear response in the range of 0.081-10.0 μg L -1 , limits detection and quantification of 0.024 and 0.081 μg L -1 , respectively; preconcentration factor of 165, consumptive index of 0.06 mL, concentration efficiency 132 min -1 , and frequency of readings equal to 26 readings h -1 The accuracy was checked by analysis of certified reference materials for trace metals and recovery tests. The obtained results were in agreement with 95% confidence level (t-test). The method was adequate to apply in samples of: jewelry (earrings) (2.38 ± 0.28 μg kg -1 ), black tea (1.09 ± 0.15 μg kg -1 ), green tea (3.85 ± 0.13 μg kg -1 ), cigarette tobacco (38.27 ± 0.22 μg kg -1 ), and hair (0.35 ± 0.02 μg kg -1 ). © The Author(s) 2016.

  6. Determination of As(III) and total inorganic As in water samples using an on-line solid phase extraction and flow injection hydride generation atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Sigrist, Mirna; Albertengo, Antonela; Beldomenico, Horacio; Tudino, Mabel

    2011-01-01

    A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH 3 generation using 3.5 mol L -1 HCl as carrier solution and 0.35% (m/v) NaBH 4 in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl - , SO 4 2- , NO 3 - , HPO 4 2- , HCO 3 - on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C 6 H 8 O 6 solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 μg L -1 and 0.6 μg L -1 for As(III) and inorganic total As, respectively, were obtained for a 500 μL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samples h -1 . The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and

  7. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

    Directory of Open Access Journals (Sweden)

    Margalida Artigues

    2017-11-01

    Full Text Available Amperometric biosensors based on the use of glucose oxidase (GOx are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%, reproducibility (RSD = 2.5%, accuracy (95–105% recovery, and robustness (RSD = 3.3%. Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

  8. N-m-nitrocinnamoylphenylhydroxyl-amine as reagent for amperometric determination of yttrium

    International Nuclear Information System (INIS)

    Oliferenko, G.L.; Gallaj, Z.A.; Sheina, N.M.; Shvedene, N.V.

    1983-01-01

    Possibility of using organic reagent of unsaturated N-arylsubstituted derivatives class of hydroxamic acids N-m-nitrocinnamoyl phenylhydroxylamire (NCPHA) for amperometric titration of yttrium using indication of e.t.p. by current of reagent oxidation on graphite electrode is investigated. Metal and the NCPHA form difficultly soluble complex with ratio of yttrium to the NCPHA, which is equal to 1:3. Buffer mixtures of 0.1MNH 3 +0.1MCH 3 COOH composis tion with pH 6.3-7.5 are optimal background solutions for amperometric titration of yttrium. The proposed method permits to determine 10-600 μkg of yttrium in the volume of 10 ml. Effect of the series of strange elements on titration of yttrium with NCPHA (Ca, Mg, Mn (2), Al, CU (2), Fe (3) REE and others) is studied. The developed method is used for yttrium determination in luminophores of Casub(n)-- Ysub(m)Fsub(z)xMn(2) (1-10%) composition

  9. A Reagentless Amperometric Formaldehyde-Selective Chemosensor Based on Platinized Gold Electrodes.

    Science.gov (United States)

    Demkiv, Olha; Smutok, Oleh; Gonchar, Mykhailo; Nisnevitch, Marina

    2017-05-06

    Fabrication and characterization of a new amperometric chemosensor for accurate formaldehyde analysis based on platinized gold electrodes is described. The platinization process was performed electrochemically on the surface of 4 mm gold planar electrodes by both electrolysis and cyclic voltamperometry. The produced electrodes were characterized using scanning electron microscopy and X-ray spectral analysis. Using a low working potential (0.0 V vs. Ag/AgCl) enabled an essential increase in the chemosensor's selectivity for the target analyte. The sensitivity of the best chemosensor prototype to formaldehyde is uniquely high (28180 A·M -1 ·m -2 ) with a detection limit of 0.05 mM. The chemosensor remained stable over a one-year storage period. The formaldehye-selective chemosensor was tested on samples of commercial preparations. A high correlation was demonstrated between the results obtained by the proposed chemosensor, chemical and enzymatic methods ( R = 0.998). The developed formaldehyde-selective amperometric chemosensor is very promising for use in industry and research, as well as for environmental control.

  10. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

    Science.gov (United States)

    2017-01-01

    Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs) has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95–105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated. PMID:29135931

  11. [Amperometric biosensor for lactate analysis in wines and grape must during fermentation].

    Science.gov (United States)

    Shkotova, L V; Horiushkina, T B; Slast'ia, E A; Soldatkin, O P; Tranh-Minh, S; Chovelon, J M; Dziadevych, S V

    2005-01-01

    The amperometric biosensor based on lactate oxidase for determination of lactate has been developed, and two methods of immobilization of lactate oxidase on the surface of industrial screen-printed platinum electrodes SensLab were compared. A sensor with immobilized in the Resydrol polymer lactate oxidase by the method of physical adsorption is characterized of narrow dynamic range and greater response value in comparison with a biosensor based on immobilised in poly(3,4-ethylenedioxythiophene) lactate oxidase by the method of electrochemical polymerization. Operational stability of the biosensor developed was studied and it was shown, that the immobilization method does not influence their stability. The analysis of the lactate in wine and during wine fermentation has been conducted. High correlation of the data obtained by means of amperometric lactate biosensor and a standard method of an ionic chromatography has been shown. The developed biosensor could be applied in the food industry for the control and optimization of the wine fermentation process, and quality control of wine.

  12. Electrochemical formation of InP porous nanostructures and its application to amperometric chemical sensors

    International Nuclear Information System (INIS)

    Sato, Taketomo; Mizohata, Akinori; Fujino, Toshiyuki; Hashizume, Tamotsu

    2008-01-01

    In this paper, we report the electrochemical formation of the InP porous nanostructures and their feasibility for the application to the amperometric chemical sensors. Our two step electrochemical process consists of the pore formation on a (001) n-type InP substrate and the subsequent etching of pore walls caused by changing the polarity of the InP electrode in a HCl-based electrolyte. By applying the anodic bias to the InP electrode, the high-density array of uniform nanopores was formed on the surface. Next, the cathodic bias was applied to the porous sample to reduce the wall thickness by cathodic decomposition of InP, where the thickness of InP nanowall decreased uniformly along the entire depth of the porous layer. From the amperometric measurements of the porous electrode, it was found that the electrocatalytic activity was much higher than that of the planar electrode. Furthermore, the current sensitivity for the H 2 O 2 detection was much enhanced after the cathodic decomposition process. The InP porous nanostructure formed by the present process is one of the promising structures for the application to the semiconductor-based bio/chemical sensors. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  13. Nonenzymatic amperometric determination of glucose by CuO nanocubes-graphene nanocomposite modified electrode.

    Science.gov (United States)

    Luo, Liqiang; Zhu, Limei; Wang, Zhenxin

    2012-12-01

    Here, we report a nonenzymatic amperometric glucose sensor based on copper oxide (CuO) nanocubes-graphene nanocomposite modified glassy carbon electrode (CuO-G-GCE). In this case, the graphene sheets were cast on the GCE directly. CuO nanocubes were obtained by oxidizing electrochemically deposited Cu on the graphene. The morphology of CuO-G nanocomposite was characterized by scanning electron microscopy. The CuO-G-GCE-based sensor exhibited excellent electrocatalytic activity and high stability for glucose oxidation. Under optimized conditions, the linearity between the current response and the glucose concentration was obtained in the range of 2μM to 4mM with a detection limit of 0.7μM (S/N=3), and a high sensitivity of 1360μAmM(-1)cm(-2). The proposed electrode showed a fast response time (less than 5s) and a good reproducibility. The as-made sensor was applied to determine the glucose levels in clinic human serum samples with satisfactory results. In addition, the effects of common interfering species, including ascorbic acid, uric acid, dopamine and other carbohydrates, on the amperometric response of the sensor were investigated and discussed in detail. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Bromopyrogallol red: a new microanalytical reagent for amperometric estimation of Dy (III) and Gd (III)

    International Nuclear Information System (INIS)

    Sahu, G.P.; Lavale, S.C.

    2000-01-01

    Bromopyrogallol red (BPR) has been extensively used as an indicator but its electro-reducibility has proved it to be a very useful amperometric reagent. BPR reduces on a DME in KNO 3 in the entire pH range 2.4 to 9.5. It produces single stage reduction wave below pH 4, but a two stage reduction wave in the basic range. Progressive ionization of hydroxyl group and distinct colour species of BPR, have also been studied using a Bausch and Lomb spectronic-20 spectrophotometer in order to support electroanalytical studies. On performing amperometric titrations of Dy(III) and Gd(III) with BPR at its plateau potential 1.0 V at pH 2.6 and μ = 0.4, reversed L-shaped titration curves have been observed indicating metal to BPR ratio 1:1 and the colour changes from claret red to orange yellow. The reagents have been tested in presence of various diverse ions and tolerance limits have been computed. Na + , K + , Li + , Cl - , ClO 4 - , CH 3 COO - , Pd 2+ , Fe 3+ ions did not interfere in the titrimetric procedure. However, small amounts of Bi 3+ , Pb 2+ , Ni 2+ , Co 2+ , Cd 2+ , Mg 2+ and rare earth metals have hampered the titrimetric estimations. (author)

  15. Amperometric morphine sensing using a molecularly imprinted polymer-modified electrode

    International Nuclear Information System (INIS)

    Yeh, W.-M.; Ho, K.-C.

    2005-01-01

    This study incorporates morphine into a molecularly imprinted polymer (MIP) for the amperometric detection of morphine. The polymer, poly(3,4-ethylenedioxythiophene), PEDOT, is an electroactive film that catalyzes morphine oxidation and lowers the oxidization potential on an indium tin oxide (ITO) electrode. The MIP-PEDOT modified electrode is prepared by electropolymerizing PEDOT onto an ITO electrode in a 0.1 M LiClO 4 solution with template addition (morphine). After template molecule extraction, the oxidizing current of the MIP-PEDOT modified electrode is measured in a 0.1 M KCl solution (pH = 5.3) at 0.75 V (versus Ag/AgCl/sat'd KCl) with the morphine concentration varying in the 0.1-5 mM range. A linear range, displaying the relationship between steady-state currents and morphine concentrations, from 0.1 to 1 mM, is obtained. The proposed amperometric sensor could be used for morphine detection with a sensitivity of 91.86 μA/cm 2 per mM. A detection limit of 0.2 mM at a signal-to-noise ratio of 3 is achieved. Moreover, the proposed method can discriminate between morphine and its analogs, such as codeine

  16. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples.

    Science.gov (United States)

    Artigues, Margalida; Abellà, Jordi; Colominas, Sergi

    2017-11-14

    Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO₂NTAs) has been evaluated. The GOx-Chitosan/TiO₂NTAs biosensor showed a sensitivity of 5.46 μA·mM -1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95-105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx-Chitosan/TiO₂NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

  17. Development of amperometric L-tyrosine sensor based on Fe-doped hydroxyapatite nanoparticles

    International Nuclear Information System (INIS)

    Kanchana, P.; Lavanya, N.; Sekar, C.

    2014-01-01

    A novel biosensor based on Fe-doped hydroxyapatite (Fe-HA) nanoparticles and tyrosinase has been developed for the detection of L-tyrosine. Nanostructured Fe-HA was synthesized by a simple microwave irradiation method, and its phase formation, morphology and magnetic property were examined by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). Electrochemical performance of the nano Fe-HA/tyrosinase modified glassy carbon electrode (GCE) for detection of L-tyrosine was investigated by cyclic voltammetry (CV) and amperometric methods. The fabricated biosensor exhibited a linear response to L-tyrosine over a wide concentration range of 1.0 × 10 −7 to 1.0 × 10 −5 M with a detection limit of 245 nM at pH 7.0. In addition, the fabricated sensor showed an excellent selectivity, good reproducibility, long-term stability and anti-interference towards the determination of L-tyrosine. - Highlights: • A novel amperometric L-tyrosine biosensor has been fabricated using nanostructured Fe-HA. • The fabricated sensor exhibits a wide linear range, good stability and high reproducibility. • Fe-HA assists microenvironment and direct electron transfer between enzyme and electrode surface. • The nano Fe-HA and electrode fabrication procedure are simple and less expensive

  18. Amperometric magnetoimmunoassay for the direct detection of tumor necrosis factor alpha biomarker in human serum

    Energy Technology Data Exchange (ETDEWEB)

    Eletxigerra, U. [Micro-NanoFabrication Unit, IK4-Tekniker, Eibar (Spain); CIC microGUNE, Arrasate-Mondragón (Spain); Martinez-Perdiguero, J. [CIC microGUNE, Arrasate-Mondragón (Spain); Merino, S. [Micro-NanoFabrication Unit, IK4-Tekniker, Eibar (Spain); CIC microGUNE, Arrasate-Mondragón (Spain); Villalonga, R.; Pingarrón, J.M. [Departamento de Química Analítica, Facultad de CC. Químicas, Universidad Complutense de Madrid, Madrid (Spain); Campuzano, S., E-mail: susanacr@quim.ucm.es [Departamento de Química Analítica, Facultad de CC. Químicas, Universidad Complutense de Madrid, Madrid (Spain)

    2014-08-01

    Highlights: • Electrochemical magnetoimmunosensor for tumor necrosis factor alpha (TNFα) biomarker. • Sensitive and selective detection of TNFα in undiluted serum. • LOD achieved lower than the cut-off value established for relevant illnesses. • Useful and affordable alternative to ELISAs for TNFα determination in serum. - Abstract: An amperometric immunoassay for the determination of tumor necrosis factor alpha (TNFα) protein biomarker in human serum based on the use of magnetic microbeads (MBs) and disposable screen-printed carbon electrodes (SPCEs) has been developed. The specifically modified microbeads were magnetically captured on the working electrode surface and the amperometric responses were measured at −0.20 V (vs. Ag pseudo-reference electrode), upon addition of hydroquinone (HQ) as electron transfer mediator and H{sub 2}O{sub 2} as the enzyme substrate. After a thorough optimization of the assay, extremely low limits of detection were achieved: 2.0 pg mL{sup −1} (36 fM) and 5.8 pg mL{sup −1} (105 fM) for standard solutions and spiked human serum, respectively. The simplicity, robustness and this clinically interesting LOD proved the developed TNFα immunoassay as a good contender for real clinical application.

  19. Amperometric magnetoimmunoassay for the direct detection of tumor necrosis factor alpha biomarker in human serum

    International Nuclear Information System (INIS)

    Eletxigerra, U.; Martinez-Perdiguero, J.; Merino, S.; Villalonga, R.; Pingarrón, J.M.; Campuzano, S.

    2014-01-01

    Highlights: • Electrochemical magnetoimmunosensor for tumor necrosis factor alpha (TNFα) biomarker. • Sensitive and selective detection of TNFα in undiluted serum. • LOD achieved lower than the cut-off value established for relevant illnesses. • Useful and affordable alternative to ELISAs for TNFα determination in serum. - Abstract: An amperometric immunoassay for the determination of tumor necrosis factor alpha (TNFα) protein biomarker in human serum based on the use of magnetic microbeads (MBs) and disposable screen-printed carbon electrodes (SPCEs) has been developed. The specifically modified microbeads were magnetically captured on the working electrode surface and the amperometric responses were measured at −0.20 V (vs. Ag pseudo-reference electrode), upon addition of hydroquinone (HQ) as electron transfer mediator and H 2 O 2 as the enzyme substrate. After a thorough optimization of the assay, extremely low limits of detection were achieved: 2.0 pg mL −1 (36 fM) and 5.8 pg mL −1 (105 fM) for standard solutions and spiked human serum, respectively. The simplicity, robustness and this clinically interesting LOD proved the developed TNFα immunoassay as a good contender for real clinical application

  20. Amperometric Enzyme-Based Biosensors for Application in Food and Beverage Industry

    Science.gov (United States)

    Csöoregi, Elisabeth; Gáspñr, Szilveszter; Niculescu, Mihaela; Mattiasson, Bo; Schuhmann, Wolfgang

    Continuous, sensitive, selective, and reliable monitoring of a large variety of different compounds in various food and beverage samples is of increasing importance to assure a high-quality and tracing of any possible source of contamination of food and beverages. Most of the presently used classical analytical methods are often requiring expensive instrumentation, long analysis times and well-trained staff. Amperometric enzyme-based biosensors on the other hand have emerged in the last decade from basic science to useful tools with very promising application possibilities in food and beverage industry. Amperometric biosensors are in general highly selective, sensitive, relatively cheap, and easy to integrate into continuous analysis systems. A successful application of such sensors for industrial purposes, however, requires a sensor design, which satisfies the specific needs of monitoring the targeted analyte in the particular application, Since each individual application needs different operational conditions and sensor characteristics, it is obvious that biosensors have to be tailored for the particular case. The characteristics of the biosensors are depending on the used biorecognition element (enzyme), nature of signal transducer (electrode material) and the communication between these two elements (electron-transfer pathway).

  1. Evaluation of different disinfectants on the performance of an on-meter dosed amperometric glucose-oxidase-based glucose meter.

    Science.gov (United States)

    Sarmaga, Don; Dubois, Jeffrey A; Lyon, Martha E

    2011-11-01

    Off-meter dosed photometric glucose-oxidase-based glucose meters have been reported to be susceptible to interference by hydrogen-peroxide-based disinfecting agents. The objective of this study was to determine if a single application of hydrogen-peroxide-containing Accel® wipe to disinfect an on-meter dosed amperometric glucose-oxidase-based glucose meter will influence its performance. The performance of five on-meter dosed amperometric glucose-oxidase-based glucose meters was determined before and after disinfecting the devices with a single application of either CaviWipes® (14.3% isopropanol and 0.23% diisobutyl-phenoxy-ethoxyethyl dimethyl benzyl ammonium chloride) or Accel (0.5% hydrogen peroxide) wipes. Replicate glucose measurements were conducted before disinfecting the devices, immediately after disinfecting, and then 1 and 2 min postdisinfecting, with measurements in triplicate. Analysis was sequentially completed for five different meters. Results were analyzed by a two-way analysis of variance (Analyze-it software). No clinical ( .05) in glucose concentration were detected when the on-meter dosed amperometric glucose-oxidase-based glucose meters were disinfected with either CaviWipes or Accel wipes and measured immediately or 1 or 2 min postdisinfecting. No clinically significant difference in glucose concentration was detected between meters (glucose oxidase amperometric-based glucose meters are not analytically susceptible to interference by a single application of hydrogen-peroxide-containing Accel disinfectant wipes. © 2011 Diabetes Technology Society.

  2. AMPEROMETRIC THICK-FILM STRIP ELECTRODES FOR MONITORING ORGANOPHOSPHATE NERVE AGENTS BASED ON IMMOBILIZED ORGANOPHOSPHORUS HYDROLASE. (R823663)

    Science.gov (United States)

    An amperometric biosensor based on the immobilization of organophosphorus hydrolase(OPH) onto screen-printed carbon electrodes is shown useful for the rapid, sensitive, and low-costdetection of organophosphate (OP) nerve agents. The sensor relies upon the sensitive and ra...

  3. In vivo continuous and simultaneous monitoring of brain energy substrates with a multiplex amperometric enzyme-based biosensor device

    NARCIS (Netherlands)

    De Lima Braga Lopes Cordeiro, Carlos; de Vries, M.G.; Ngabi, W; Oomen, P.E.; Cremers, T.I.F.H.; Westerink, B.H.C.

    2015-01-01

    Enzyme-based amperometric biosensors are widely used for monitoring key biomarkers. In experimental neuroscience there is a growing interest in in vivo continuous and simultaneous monitoring of metabolism-related biomarkers, like glucose, lactate and pyruvate. The use of multiplex biosensors will

  4. Acceleration effect of alcohols on ion association of molbdophosphate with malachite green and its use to the sensitive flow-injection determination of phosphate. Molybdo rinsan ion-malachite green ion kaigotai seisei ni oyobosu alcohol no hanno sokushinkoka to sore wo riyosuru rin no kokando flow injection bunseki

    Energy Technology Data Exchange (ETDEWEB)

    Motomizu, S; Yasuda, Y; Oshima, M [Okayama Univ., Okayama (Japan). Faculty of Science

    1991-12-10

    Molibdophosphoric acid (PMo) reacts with malachite green (MG{sup +}) to form a colored ion associate (MG{sup +}- PMo) in an acidic solution according to the formula : HMG{sup 2+}+H{sub 3}PMo{sub 12}O{sub 40}{yields}(MG{sup +})H{sub 2}PMo{sub 12}O{sub 40}+2H{sup +}. A protonated form HMG{sup 2+} is yellow (the absorption mximum at 446 nm), whereas the ion associate MG{sup +} is blue green (the absorption maximum at 650 nm). MG{sup +} is found to accelerate the formation of PMo. Water-miscible organic solvents such as methanol,ethanol and propanol also accelerate the formation of PMo as well as the formation of MG sup + - PMo. Some anionic surfactants decelerate the reaction, however, contribute to the suppression of the baseline drift in a flow injection analysis (FIA). By the use of the proposed reaction accelerator and surfactant. a highly sensitive FIA system is established for,orthophosphate up to the range of several ppb. 16 figs.. 11 refs.

  5. Photometric flow injection determination of phosphate on a PDMS microchip using an optical detection system assembled with an organic light emitting diode and an organic photodiode.

    Science.gov (United States)

    Liu, Rong; Ishimatsu, Ryoichi; Yahiro, Masayuki; Adachi, Chihaya; Nakano, Koji; Imato, Toshihiko

    2015-01-01

    and a good linear relationship between the concentration and absorbance was observed in the concentration range 0-0.2 ppm, with a detection limit (S/N=3) of 0.02 ppm. The assembled photometric detector was also applied to the determination of phosphate by the flow injection of river water samples using the reagent solution containing MG and molybdenum ammonium in sulfuric acid. A good recovery (97-99%) for the river water samples, which had been spiked with the standard 0.08 ppm, with an RSD of ca 5% (n=5) was obtained using the constructed system. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Flow-injection spectrophotometric determination of captopril in pharmaceutical formulations using a new solid-phase reactor containing AgSCN immobilized in a polyurethane resin

    Directory of Open Access Journals (Sweden)

    Fernando Campanhã Vicentini

    2012-06-01

    Full Text Available A simple flow-injection analysis procedure was developed for determining captopril in pharmaceutical formulations employing a novel solid-phase reactor containing silver thiocyanate immobilized in a castor oil derivative polyurethane resin. The method was based on silver mercaptide formation between the captopril and Ag(I in the solid-phase reactor. During such a reaction, the SCN- anion was released and reacted with Fe3+, which generated the FeSCN2+ complex that was continuously monitored at 480 nm. The analytical curve was linear in the captopril concentration range from 3.0 × 10-4 mol L-1 to 1.1 × 10-3 mol L-1 with a detection limit of 8.0 × 10-5 mol L-1. Recoveries between 97.5% and 103% and a relative standard deviation of 2% for a solution containing 6.0 × 10-4 mol L-1 captopril (n = 12 were obtained. The sample throughput was 40 h-1 and the results obtained for captopril in pharmaceutical formulations using this procedure and those obtained using a pharmacopoeia procedure were in agreement at a 95% confidence level.Um procedimento simples de análise por injeção em fluxo foi desenvolvido para a determinação de captopril em formulações farmacêuticas empregando um novo reator em fase sólida contendo tiocianato de prata imobilizado em resina poliuretana obtida a partir de óleo de mamona. O método foi baseado na formação de um mercapto composto de prata, no reator em fase sólida, obtido entre o captopril e Ag (I imobilizada. Durante a reação, íons SCN- eram liberados e reagiam com Fe3+, gerando o complexo FeSCN2+, que foi continuamente monitorado em 480 nm. A curva analítica foi linear no intervalo de concentração de captopril entre 3,0 × 10-4 a 1,1 × 10-3 mol L-1 com um limite de detecção de 8,0 × 10-5 mol L-1. Recuperações entre 97,5-103% e desvio padrão relativo de 2% para uma solução contendo 6,0 × 10-4 mol L-1 de captopril (n = 12 foram obtidos. A frequência de amostragem foi de 40 h-1 e os resultados

  7. Selective Flow-Injection Quantification of Ultra-trace Amounts of Cr(VI) via On-line Complexation and Preconcentration with APDC Followed by Determination by Electrothermal Atomic Absorption Spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Steffen; Hansen, Elo Harald

    1998-01-01

    A rapid, sensitive and selective time-based flow injection (FI) preconcentration procedure is described for the determination of ultra-trace amounts of Cr(VI) via on-line reaction with ammonium pyrrolidine dithiocarbamate (APDC) and formation of the Cr(VI)-PDC complex. The preconcentration...... to direct introduction of 55 mu l samples, yielding a detection limit (3 sigma) of 4.2 ng l(-1). The sample frequency was 21.2 samples per hour. The proposed method was evaluated by analyzing drinking water, a NIST Cr(VI)-reference material and synthetic sea water. A major contribution to successful...

  8. Prussian blue-modified nanoporous gold film electrode for amperometric determination of hydrogen peroxide.

    Science.gov (United States)

    Ghaderi, Seyran; Mehrgardi, Masoud Ayatollahi

    2014-08-01

    In this manuscript, the electrocatalytic reduction of hydrogen peroxides on Prussian blue (PB) modified nanoporous gold film (NPGF) electrode is described. The PB/NPGF is prepared by simple anodizing of a smooth gold film followed by PB film electrodeposition method. The morphology of the PB/NPGF electrode is characterized using scanning electron microscopy (SEM). The effect of solution pH and the scan rates on the voltammetric responses of hydrogen peroxide have also been examined. The amperometric determination of H2O2 shows two linear dynamic responses over the concentration range of 1μM-10μM and 10μM-100μM with a detection limit of 3.6×10(-7)M. Furthermore, this electrode demonstrated good stability, repeatability and selectivity remarkably. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Amperometric estimation of La3+ and Ce3+ with cupferron using d.m.e

    International Nuclear Information System (INIS)

    Pitre, K.S.; Lavale, S.C.

    1982-01-01

    Cupferron has been employed as a reagent for the amperometric titrations of La 3+ and Ce 3+ in very dilute solution using d.m.e. Hydrochloric acid (pH=2.75) has been used as supporting electrolyte. These titrations revealed cupferron to metal ratio of 1:1. Titrations are not hampered by the presence of a fairly large amount of Li + , Na + , K + , Mg 3+ , Zn 3+ , Al 3+ , Cl - , Br - , I - , NO 3 - , NO 2 - , CH 2 COO - and ClO 4 - ions. Furthermore, micro and ultramicro quantities of La 3+ and Ce 2+ have been successfully determined with an error of less than +- 0.70%. (author)

  10. Determination of carbohydrates by high performance anion chromatography-pulsed amperometric detection in mushrooms.

    Science.gov (United States)

    Zhou, Shuai; Tang, Qingjiu; Luo, Xi; Xue, Jun-Jie; Liu, Yanfang; Yang, Yan; Zhang, Jingsong; Feng, Na

    2012-01-01

    A method of detecting carbohydrates (fucose, trehalose, mannitol, arabitol, mannose, glucose, galactose, fructose, and ribose) by high-performance anion chromatography-pulsed amperometric detection (HAPEC-PAD) was established. The conditions are: CarboPac MA1 column, NaOH as the eluent, temperature 30°C, Au working electrode, Ag/AgCl reference electrode, and flow rate 0.4 mL/min. These nine analytes, which yielded high resolution by this method, could be detected in 40 minutes. Mushrooms were tested and good precision, stability, and reproducibility were achieved. This method is suitable for mushroom samples and could support research and development on sugar and sugar alcohol, which contains special effects.

  11. Determination of carbohydrates using pulsed amperometric detection combined with anion exchange separations

    Energy Technology Data Exchange (ETDEWEB)

    Edwards, W.T.; Pohl, C.A.; Rubin, R.

    1987-06-01

    Carbohydrates, including the monosaccharides commonly found in wood and wood pulp hydrolyzates, are separated by anion exchange chromatography using hydroxide and acetate eluants and are determined using pulsed amperometric detection. The detection method is based on oxidizing the sugars in a flow-through electrochemical cell equipped with a gold working electrode. A repeating cycle of three potentials is used: the first to oxidize the carbohydrates and measure the current generated, and two subsequent pulses to clean the electrode surface of oxidation products. The method is fast, sensitive, and requires no pre-column derivatization. It is applied to a sample of hydrolyzed wood pulp, which can be analyzed after minimal sample preparation. Detection limits are of the order of 1 mg/kg for monosaccharides in a 50 micro L injection. (Refs. 8).

  12. Amperometric Morphine Detection Using Pt-Co Alloy Nanowire Array-modified Electrode

    International Nuclear Information System (INIS)

    Tao, Manlan; Xu, Feng; Li, Yueting; Xu, Quanqing; Chang, Yanbing; Yang, Yunhui; Wu, Zaisheng

    2010-01-01

    Pt-Co alloy nanowire array was directly synthesized by electrochemical deposition with polycarbonate template at -1.0V and subsequent chemical etching of the template. The use of Pt-Co alloy nanowire array-modified electrode (Pt- Co NAE) for the determination of morphine (MO) is described. The morphology of the Pt-Co alloy nanowire array has been investigated by scanning electron microscopy (SEM) and energy disperse X-ray spectroscopy (EDS) analysis), respectively. The resulting Pt-Co NAE offered a linear amperometric response for morphine ranging from 2.35 x 10 -5 to 2.39 x 10 -3 M with a detection limit of 7.83 x 10 -6 M at optimum conditions. This sensor displayed high sensitivity and long-term stability

  13. Amperometric Biosensor for Monitoring Respiration Activity of Saccharomyces cerevisiae in the Presence of Cobalt and Zinc

    Directory of Open Access Journals (Sweden)

    Miroslav Mikšaj

    2002-01-01

    Full Text Available For efficient control of heavy metal concentrations electrochemical methods, such as polarography and related techniques, are applied. Their advantages are simplicity, short analysis time and small quantities of samples needed. The presence of some heavy metals, such as zinc and cobalt, accelerates the growth of yeast. For the measurements of concentration changes, amperometric biosensor containing yeast Saccharomyces cerevisiae was used. The influence of zinc and cobalt on respiratory activity of the yeast Saccharomyces cerevisiae was estimated by measuring oxygen in the solution that was earlier enriched with cobalt or zinc. Measurements were performed using modified Clark’s oxygen electrode and the investigated concentrations of cobalt and zinc were up to 100 mg/L.

  14. An Amperometric Biosensor for Uric Acid Determination Prepared From Uricase Immobilized in Polyaniline-Polypyrrole Film

    Directory of Open Access Journals (Sweden)

    Fatma Arslan

    2008-09-01

    Full Text Available A new amperometric uric acid biosensor was developed by immobilizing uricase by a glutaraldehyde crosslinking procedure on polyaniline-polypyrrole (pani-ppy composite film on the surface of a platinum electrode. Determination of uric acid was performed by the oxidation of enzymatically generated H2O2 at 0.4 V vs. Ag/AgCl. The linear working range of the biosensor was 2.5×10-6 – 8.5×10-5 M and the response time was about 70 s. The effects of pH, temperature were investigated and optimum parameters were found to be 9.0, 55 oC, respectively. The stability and reproducibility of the enzyme electrode have been also studied.

  15. A CMOS analog front-end chip for amperometric electrochemical sensors

    International Nuclear Information System (INIS)

    Li Zhichao; Chen Min; Xiao Jingbo; Chen Jie; Liu Yuntao

    2015-01-01

    This paper reports a complimentary metal–oxide–semiconductor (CMOS) analog front-end chip for amperometric electrochemical sensors. The chip includes a digital configuration circuit, which can communicate with an external microcontroller by employing an I 2 C interface bus, and thus is highly programmable. Digital correlative double samples technique and an incremental sigma–delta analog to digital converter (Σ–Δ ADC) are employed to achieve a new proposed system architecture with double samples. The chip has been fabricated in a standard 0.18-μm CMOS process with high-precision and high-linearity performance occupying an area of 1.3 × 1.9 mm 2 . Sample solutions with various phosphate concentrations have been detected with a step concentration of 0.01 mg/L. (paper)

  16. Amperometric nitrate biosensor based on Carbon nanotube/Polypyrrole/Nitrate reductase biofilm electrode

    Energy Technology Data Exchange (ETDEWEB)

    Can, Faruk; Korkut Ozoner, Seyda; Ergenekon, Pinar; Erhan, Elif, E-mail: e.erhan@gyte.edu.tr

    2012-01-01

    This study describes the construction and characterization of an amperometric nitrate biosensor based on the Polypyrrole (PPy)/Carbon nanotubes (CNTs) film. Nitrate reductase (NR) was both entrapped into the growing PPy film and chemically immobilized via the carboxyl groups of CNTs to the CNT/PPy film electrode. The optimum amperometric response for nitrate was obtained in 0.1 M phosphate buffer solution (PBS), pH 7.5 including 0.1 M lithium chloride and 7 mM potassium ferricyanide with an applied potential of 0.13 V (vs. Ag/AgCl, 3 M NaCl). Sensitivity was found to be 300 nA/mM in a linear range of 0.44-1.45 mM with a regression coefficient of 0.97. The biosensor response showed a higher linear range in comparison to standard nitrate analysis methods which were tested in this study and NADH based nitrate biosensors. A minimum detectable concentration of 0.17 mM (S/N = 3) with a relative standard deviation (RSD) of 5.4% (n = 7) was obtained for the biosensor. Phenol and glucose inhibit the electrochemical reaction strictly at a concentration of 1 {mu}g/L and 20 mg/L, respectively. The biosensor response retained 70% of its initial response over 10 day usage period when used everyday. - Highlights: Black-Right-Pointing-Pointer K{sub 3}Fe(CN){sub 6} has been used for the first time as mediator for nitrate reductase. Black-Right-Pointing-Pointer Better performance was obtained in comparison to other nitrate biosensor studies operated with various mediators. Black-Right-Pointing-Pointer Analytical parameters were better than standard nitrate analysis methods.

  17. Amperometric nitrate biosensor based on Carbon nanotube/Polypyrrole/Nitrate reductase biofilm electrode

    International Nuclear Information System (INIS)

    Can, Faruk; Korkut Ozoner, Seyda; Ergenekon, Pinar; Erhan, Elif

    2012-01-01

    This study describes the construction and characterization of an amperometric nitrate biosensor based on the Polypyrrole (PPy)/Carbon nanotubes (CNTs) film. Nitrate reductase (NR) was both entrapped into the growing PPy film and chemically immobilized via the carboxyl groups of CNTs to the CNT/PPy film electrode. The optimum amperometric response for nitrate was obtained in 0.1 M phosphate buffer solution (PBS), pH 7.5 including 0.1 M lithium chloride and 7 mM potassium ferricyanide with an applied potential of 0.13 V (vs. Ag/AgCl, 3 M NaCl). Sensitivity was found to be 300 nA/mM in a linear range of 0.44–1.45 mM with a regression coefficient of 0.97. The biosensor response showed a higher linear range in comparison to standard nitrate analysis methods which were tested in this study and NADH based nitrate biosensors. A minimum detectable concentration of 0.17 mM (S/N = 3) with a relative standard deviation (RSD) of 5.4% (n = 7) was obtained for the biosensor. Phenol and glucose inhibit the electrochemical reaction strictly at a concentration of 1 μg/L and 20 mg/L, respectively. The biosensor response retained 70% of its initial response over 10 day usage period when used everyday. - Highlights: ► K 3 Fe(CN) 6 has been used for the first time as mediator for nitrate reductase. ► Better performance was obtained in comparison to other nitrate biosensor studies operated with various mediators. ► Analytical parameters were better than standard nitrate analysis methods.

  18. Real-Time Telemetry System for Amperometric and Potentiometric Electrochemical Sensors

    Directory of Open Access Journals (Sweden)

    Ching-Hsing Luo

    2011-09-01

    Full Text Available A real-time telemetry system, which consists of readout circuits, an analog-to-digital converter (ADC, a microcontroller unit (MCU, a graphical user interface (GUI, and a radio frequency (RF transceiver, is proposed for amperometric and potentiometric electrochemical sensors. By integrating the proposed system with the electrochemical sensors, analyte detection can be conveniently performed. The data is displayed in real-time on a GUI and optionally uploaded to a database via the Internet, allowing it to be accessed remotely. An MCU was implemented using a field programmable gate array (FPGA to filter noise, transmit data, and provide control over peripheral devices to reduce power consumption, which in sleep mode is 70 mW lower than in operating mode. The readout circuits, which were implemented in the TSMC 0.18-μm CMOS process, include a potentiostat and an instrumentation amplifier (IA. The measurement results show that the proposed potentiostat has a detectable current range of 1 nA to 100 μA, and linearity with an R2 value of 0.99998 in each measured current range. The proposed IA has a common-mode rejection ratio (CMRR greater than 90 dB. The proposed system was integrated with a potentiometric pH sensor and an amperometric nitrite sensor for in vitro experiments. The proposed system has high linearity (an R2 value greater than 0.99 was obtained in each experiment, a small size of 5.6 cm × 8.7 cm, high portability, and high integration.

  19. Determination of ammonium ion using a reagentless amperometric biosensor based on immobilized alanine dehydrogenase.

    Science.gov (United States)

    Tan, Ling Ling; Musa, Ahmad; Lee, Yook Heng

    2011-01-01

    The use of the enzyme alanine dehydrogenase (AlaDH) for the determination of ammonium ion (NH(4)(+)) usually requires the addition of pyruvate substrate and reduced nicotinamide adenine dinucleotide (NADH) simultaneously to effect the reaction. This addition of reagents is inconvenient when an enzyme biosensor based on AlaDH is used. To resolve the problem, a novel reagentless amperometric biosensor using a stacked methacrylic membrane system coated onto a screen-printed carbon paste electrode (SPE) for NH(4)(+) ion determination is described. A mixture of pyruvate and NADH was immobilized in low molecular weight poly(2-hydroxyethyl methacrylate) (pHEMA) membrane, which was then deposited over a photocured pHEMA membrane (photoHEMA) containing alanine dehydrogenase (AlaDH) enzyme. Due to the enzymatic reaction of AlaDH and the pyruvate substrate, NH(4)(+) was consumed in the process and thus the signal from the electrocatalytic oxidation of NADH at an applied potential of +0.55 V was proportional to the NH(4)(+) ion concentration under optimal conditions. The stacked methacrylate membranes responded rapidly and linearly to changes in NH(4)(+) ion concentrations between 10-100 mM, with a detection limit of 0.18 mM NH(4)(+) ion. The reproducibility of the amperometrical NH(4)(+) biosensor yielded low relative standard deviations between 1.4-4.9%. The stacked membrane biosensor has been successfully applied to the determination of NH(4)(+) ion in spiked river water samples without pretreatment. A good correlation was found between the analytical results for NH(4)(+) obtained from the biosensor and the Nessler spectrophotometric method.

  20. Application of a field flow preconcentration system with a minicolumn packed with amberlite XAD-4/1-(2-pyridylazo)-2-naphtol and a flow injection-flame atomic adsorption spectrometric system for lead determination in sea water

    International Nuclear Information System (INIS)

    Carmen Yebra, M. del; Rodriguez, L.; Puig, L.; Moreno-Cid, A.

    2002-01-01

    A field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 1-(2-pyridylazo)-2-naphthol was used to preconcentrate lead from seawater. Elution of retained lead on the minicolumns was performed by a flow-injection-flame atomic absorption spectrometric system. Factorial designs have been used to optimize the field flow preconcentration system and the flow injection elution process. Factors such as sample pH, sample flow-rate, eluent concentration and volume (hydrochloric acid), elution flow-rate and minicolumn diameter were considered. The results suggest that the sample flow-rate and the eluent volume are statistically significant factors. The detection limit (3σ) of the procedure was 5 ng/L for a sample volume of 1000 ml. The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 4.0-3.1 % in lead solutions of 50-200 ng/L. This procedure has been successfully applied to the determination of lead in seawater from Galicia (Spain). (author)

  1. A simple and sensitive flow injection method based on the catalytic activity of CdS quantum dots in an acidic permanganate chemiluminescence system for determination of formaldehyde in water and wastewater.

    Science.gov (United States)

    Khataee, Alireza; Lotfi, Roya; Hasanzadeh, Aliyeh; Iranifam, Mortaza

    2016-04-01

    A simple and sensitive flow injection chemiluminescence (CL) method in which CdS quantum dots (QDs) enhanced the CL intensity of a KMnO4-formaldehyde (HCHO) reaction was offered for the determination of HCHO. This CL system was based on the catalytic activity of CdS QDs and their participation in the CL resonance energy transfer (CRET) phenomenon. A possible mechanism for the supplied CL system was proposed using the kinetic curves of the CL systems and the spectra of CL, photoluminescence (PL) and ultraviolet-visible (UV-Vis). The emanated CL intensity of the KMnO4-CdS QDs system was amplified in the presence of a trace level of HCHO. Based on this enhancement effect, a simple and sensitive flow injection CL method was suggested for the determination of HCHO concentration in environmental water and wastewater samples. Under selected optimized experimental conditions, the increased CL intensity was proportional to the HCHO concentration in the range of 0.03-4.5 μg L(-1) and 4.5-10.0 μg L(-1). The detection limits (3σ) were 0.0003 μg L(-1) and 1.2 μg L(-1). The relative standard deviations (RSD%) for eleven replicate determinations of 4.0 μg L(-1) HCHO were 2.2%. Furthermore, the feasibility of the developed method was investigated via the determination of HCHO concentration in environmental water and wastewater samples.

  2. Simultaneous detection of selenium by atomic fluorescence and sulfur by molecular emission by flow-injection hydride generation with on-line reduction for the determination of selenate, sulfate and sulfite

    Energy Technology Data Exchange (ETDEWEB)

    Tyson, J.F., E-mail: tyson@chem.umass.edu [Department of Chemistry, University of Massachusetts, 710 North Pleasant Street, Amherst, MA 01003 (United States); Palmer, C.D. [Lead Poisoning Trace Elements Laboratory, Wadsworth Center, New York State Department of Health, P.O. Box 509, Empire State Plaza, Albany, NY 12201-0509 (United States)

    2009-10-12

    An inductively coupled plasma atomic fluorescence spectrometry (ICP-AFS) instrument, was modified so that it was capable of monitoring transient chromatographic or flow-injection profiles and that sulfur molecular emission and selenium atomic fluorescence could be monitored simultaneously in an argon-hydrogen diffusion flame on a glass burner. The analytes were introduced as hydrogen selenide and hydrogen sulfide, generated on a flow-injection manifold. Selenate was reduced to hydride-forming selenite by microwave-assisted on-line reaction with hydrochloric acid, and sulfate, or sulfite, was reduced to hydride-forming sulfide by a mixture of hydriodic acid, acetic acid and sodium hypophosphite. The effects of the nature of reducing agent, flow rate, microwave power and coil length were studied. The limit of detection (3 s) for selenium was 10 {mu}g L{sup -1}, and for sulfide was 70 {mu}g L{sup -1} (200-{mu}L injection volume). The calibration was linear for selenium up to 2 mg L{sup -1} and to 10 mg L{sup -1} for sulfide. The throughput was 180 h{sup -1}. The three sulfur species could be differentiated on the basis of reactivity at various microwave powers.

  3. Parallel synthesis of libraries of anodic and cathodic functionalized electrodeposition paints as immobilization matrix for amperometric biosensors.

    Science.gov (United States)

    Ngounou, Bertrand; Aliyev, Elchin H; Guschin, Dmitrii A; Sultanov, Yusif M; Efendiev, Ayaz A; Schuhmann, Wolfgang

    2007-09-01

    The integration of flexible anchoring groups bearing imidazolyl or pyridyl substituents into the structure of electrodeposition paints (EDP) is the basis for the parallel synthesis of a library containing 107 members of different cathodic and anodic EDPs with a high variation in polymer properties. The obtained EDPs were used as immobilization matrix for biosensor fabrication using glucose oxidase as a model enzyme. Amperometric glucose sensors based on the different EDPs showed a wide variation in their sensor characteristics with respect to the apparent Michaelis-Menten constant (KM(app)) representing the linear measuring range and the maximum current (Imax(app)). Based on these results first assumptions concerning the impact of different side chains in the EDP on the expected biosensor properties could be obtained allowing for an improved rational optimization of EDPs used as immobilization matrix in amperometric biosensors.

  4. Application of L-lactate-cytochrome c-oxidoreductase for development of amperometric biosensor for L-lactate determination

    Directory of Open Access Journals (Sweden)

    Dzyadevych S. V.

    2009-06-01

    Full Text Available Aim. Development of amperometric biosensor based on L-lactate-cytochrome c-oxidoreductase (flavocytochrome b2, FC b2 for lactate determination. Methods. All experiments were performed using the amperometric method of detection. The methods of electrochemical polymerization and immobilization in glutaraldehyde vapors were used for FC b2 immobilization on the surface of electrodes. Results. The FC b2 preparation, which demonstrated the best operational characteristics after immobilization in poly (3,4-ethylen dioxythiophene, was selected. The selectivity, operational and storage stability, and pH-optimum for operation of the created biosensor were determined. The analysis of L-lactate in the model solutions and wine samples was carried outusing the developed biosensor. Conclusion. The FC b2-based biosensor due to its high stability can be effectively used for lactate determination in blood and other liquids containing no ethanol. After the selectivity optimization, the devise can be also applied for wine analysis.

  5. Optimization of Glucose oxidase towards oxygen independency and high mediator activity for amperometric glucose determination in diabetes analytics

    OpenAIRE

    Arango Gutierrez, Erik Uwe

    2015-01-01

    Glucose oxidase is an oxidoreductase exhibiting a high β-D-glucose specificity and high stability which renders glucose oxidase well-suited for applications in diabetes care. Nevertheless, GOx activity is highly oxygen dependent which can lead to inaccuracies in amperometric β-D-glucose determinations. Therefore a directed evolution campaign with two rounds of random mutagenesis (SeSaM followed by epPCR), site saturation mutagenesis studies, and one simultaneous site saturation library (OmniC...

  6. Amperometric Ion-Selective Electrode for Alkali Metal Cations Based on a Room-Temperature Ionic Liquid Membrane

    Czech Academy of Sciences Publication Activity Database

    Langmaier, Jan; Trojánek, Antonín; Samec, Zdeněk

    2009-01-01

    Roč. 21, 17-18 (2009), s. 1977-1983 ISSN 1040-0397 R&D Projects: GA MŠk ME08098; GA AV ČR IAA400400704 Institutional research plan: CEZ:AV0Z40400503 Keywords : room-temperature ionic liquid * alkali metals * Crown ether * cyclic voltammetry * amperometric ion-selective elkectrode Subject RIV: CG - Electrochemistry Impact factor: 2.630, year: 2009

  7. Bioethanol in Biofuels Checked by an Amperometric Organic Phase Enzyme Electrode (OPEE Working in “Substrate Antagonism” Format

    Directory of Open Access Journals (Sweden)

    Mauro Tomassetti

    2016-08-01

    Full Text Available The bioethanol content of two samples of biofuels was determined directly, after simple dilution in decane, by means of an amperometric catalase enzyme biosensor working in the organic phase, based on substrate antagonisms format. The results were good from the point of view of accuracy, and satisfactory for what concerns the recovery test by the standard addition method. Limit of detection (LOD was on the order of 2.5 × 10−5 M.

  8. Modification of alumina matrices through chemical etching and electroless deposition of nano-Au array for amperometric sensing

    Directory of Open Access Journals (Sweden)

    Valinčius Gintaras

    2007-01-01

    Full Text Available AbstractSimple nanoporous alumina matrix modification procedure, in which the electrically highly insulating alumina barrier layer at the bottom of the pores is replaced with the conductive layer of the gold beds, was described. This modification makes possible the direct electron exchange between the underlying aluminum support and the redox species encapsulated in the alumina pores, thus, providing the generic platform for the nanoporous alumina sensors (biosensors with the direct amperometric signal readout fabrication.

  9. A LabVIEW®-based software for the control of the AUTORAD platform. A fully automated multisequential flow injection analysis Lab-on-Valve (MSFIA-LOV) system for radiochemical analysis

    International Nuclear Information System (INIS)

    Barbesi, Donato; Vilas, Victor Vicente; Millet, Sylvain; Sandow, Miguel; Colle, Jean-Yves; Heras, Laura Aldave de las

    2017-01-01

    A LabVIEW®-based software for the control of the fully automated multi-sequential flow injection analysis Lab-on-Valve (MSFIA-LOV) platform AutoRAD performing radiochemical analysis is described. The analytical platform interfaces an Arduino®-based device triggering multiple detectors providing a flexible and fit for purpose choice of detection systems. The different analytical devices are interfaced to the PC running LabVIEW®VI software using USB and RS232 interfaces, both for sending commands and receiving confirmation or error responses. The AUTORAD platform has been successfully applied for the chemical separation and determination of Sr, an important fission product pertinent to nuclear waste. (author)

  10. A LabVIEW®-based software for the control of the AUTORAD platform: a fully automated multisequential flow injection analysis Lab-on-Valve (MSFIA-LOV) system for radiochemical analysis.

    Science.gov (United States)

    Barbesi, Donato; Vicente Vilas, Víctor; Millet, Sylvain; Sandow, Miguel; Colle, Jean-Yves; Aldave de Las Heras, Laura

    2017-01-01

    A LabVIEW ® -based software for the control of the fully automated multi-sequential flow injection analysis Lab-on-Valve (MSFIA-LOV) platform AutoRAD performing radiochemical analysis is described. The analytical platform interfaces an Arduino ® -based device triggering multiple detectors providing a flexible and fit for purpose choice of detection systems. The different analytical devices are interfaced to the PC running LabVIEW ® VI software using USB and RS232 interfaces, both for sending commands and receiving confirmation or error responses. The AUTORAD platform has been successfully applied for the chemical separation and determination of Sr, an important fission product pertinent to nuclear waste.

  11. Coupling on-line preconcentration by ion-exchange with ETAAS. A novel flow injection approach based on the use of a renewable microcolumn as demonstrated for the determination of nickel in environmental and biological samples

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2000-01-01

    microcolumn incorporated within an integrated micro FI-system, the column is loaded with a defined volume of small beads of an SP Sephadex C-25 cation-exchange resin and subsequently exposed to a metered amount of sample solution. However, instead of eluting the retained analyte from the organic ion-exchange......A novel way of exploiting flow injection/sequential injection (FIA/SIA) on-line ion-exchange preconcentration with detection by electrothermal atomic absorption spectrometry (ETAAS) is described and demonstrated for the determination of trace-levels of nickel. Based on the use of a renewable...... resin, the beads are along with 30 mul of carrier (buffer) solution transported via air segmentation directly into the graphite tube, where they are ashed during the pyrolysis and atomization process. The ETAAS determination is performed in parallel with the preconcentration process of the ensuing...

  12. Real-Time Amperometric Recording of Extracellular H2O2 in the Brain of Immunocompromised Mice: An In Vitro, Ex Vivo and In Vivo Characterisation Study

    Science.gov (United States)

    Reid, Caroline H.; Finnerty, Niall J.

    2017-01-01

    We detail an extensive characterisation study on a previously described dual amperometric H2O2 biosensor consisting of H2O2 detection (blank) and degradation (catalase) electrodes. In vitro investigations demonstrated excellent H2O2 sensitivity and selectivity against the interferent, ascorbic acid. Ex vivo studies were performed to mimic physiological conditions prior to in vivo deployment. Exposure to brain tissue homogenate identified reliable sensitivity and selectivity recordings up to seven days for both blank and catalase electrodes. Furthermore, there was no compromise in pre- and post-implanted catalase electrode sensitivity in ex vivo mouse brain. In vivo investigations performed in anaesthetised mice confirmed the ability of the H2O2 biosensor to detect increases in amperometric current following locally perfused/infused H2O2 and antioxidant inhibitors mercaptosuccinic acid and sodium azide. Subsequent recordings in freely moving mice identified negligible effects of control saline and sodium ascorbate interference injections on amperometric H2O2 current. Furthermore, the stability of the amperometric current was confirmed over a five-day period and analysis of 24-h signal recordings identified the absence of diurnal variations in amperometric current. Collectively, these findings confirm the biosensor current responds in vivo to increasing exogenous and endogenous H2O2 and tentatively supports measurement of H2O2 dynamics in freely moving NOD SCID mice. PMID:28698470

  13. A Differential Electrochemical Readout ASIC With Heterogeneous Integration of Bio-Nano Sensors for Amperometric Sensing.

    Science.gov (United States)

    Ghoreishizadeh, Sara S; Taurino, Irene; De Micheli, Giovanni; Carrara, Sandro; Georgiou, Pantelis

    2017-10-01

    A monolithic biosensing platform is presented for miniaturized amperometric electrochemical sensing in CMOS. The system consists of a fully integrated current readout circuit for differential current measurement as well as on-die sensors developed by growing platinum nanostructures (Pt-nanoS) on top of electrodes implemented with the top metal layer. The circuit is based on the switch-capacitor technique and includes pseudodifferential integrators for concurrent sampling of the differential sensor currents. The circuit further includes a differential to single converter and a programmable gain amplifier prior to an ADC. The system is fabricated in [Formula: see text] technology and measures current within [Formula: see text] with minimum input-referred noise of [Formula: see text] and consumes [Formula: see text] from a [Formula: see text] supply. Differential sensing for nanostructured sensors is proposed to build highly sensitive and offset-free sensors for metabolite detection. This is successfully tested for bio-nano-sensors for the measurement of glucose in submilli molar concentrations with the proposed readout IC. The on-die electrodes are nanostructured and cyclic voltammetry run successfully through the readout IC to demonstrate detection of [Formula: see text].

  14. An amperometric enzyme biosensor for real-time measurements of cellobiohydrolase activity on insoluble cellulose

    DEFF Research Database (Denmark)

    Cruys-Bagger, Nicolaj; Guilin, Ren; Tatsumi, Hirosuke

    2012-01-01

    An amperometric enzyme biosensor for continuous detection of cellobiose has been implemented as an enzyme assay for cellulases. We show that the initial kinetics for cellobiohydrolase I, Cel7A from Trichoderma reesei, acting on different types of cellulose substrates, semi-crystalline and amorphous......, can be monitored directly and in real-time by an enzyme-modified electrode based on cellobiose dehydrogenase (CDH) from Phanerochaete chrysosporium (Pc). PcCDH was cross-linked and immobilized on the surface of a carbon paste electrode which contained a mediator, benzoquinone. An oxidation current...... of the reduced mediator, hydroquinone, produced by the CDH-catalyzed reaction with cellobiose, was recorded under constant-potential amperometry at +0.5 V (vs. Ag/AgCl). The CDH-biosensors showed high sensitivity (87.7 µA mM−1 cm−2), low detection limit (25 nM), and fast response time (t95% ∼ 3 s...

  15. Amperometric biosensor for hydrogen peroxide based on hemoglobin entrapped in titania sol-gel film

    International Nuclear Information System (INIS)

    Yu Jiuhong; Ju Huangxian

    2003-01-01

    Hemoglobin (Hb) was entrapped in a titania sol-gel matrix and used as a mimetic peroxidase to construct a novel amperometric biosensor for hydrogen peroxide. The Hb entrapped titania sol-gel film was obtained with a vapor deposition method, which simplified the traditional sol-gel process for protein immobilization. The morphologies of both titania sol-gel and the Hb films were characterized using scanning electron microscopy (SEM) and proved to be chemically clean, porous, homogeneous. This matrix provided a biocompatible microenvironment for retaining the native structure and activity of the entrapped Hb and a very low mass transport barrier to the substrates. H 2 O 2 could be reduced by the catalysis of the entrapped hemoglobin at -300 mV without any mediator. The reagentless H 2 O 2 sensor exhibited a fast response (less than 5 s) and sensitivity as high as 1.29 mA mM -1 cm -2 . The linear range for H 2 O 2 determination was from 5.0x10 -7 to 5.4x10 -5 M with a detection limit of 1.2x10 -7 M. The apparent Michaelis-Menten constant of the encapsulated hemoglobin was calculated to be 0.18±0.02 mM. The stability of the biosensor was also evaluated

  16. Preparation of cholesterol oxidase nanoparticles and their application in amperometric determination of cholesterol

    Energy Technology Data Exchange (ETDEWEB)

    Chawla, Sheetal; Rawal, Rachna; Sonia; Ramrati; Pundir, C. S., E-mail: pundircs@rediffmail.com [M. D. University, Department of Biochemistry (India)

    2013-09-15

    The nanoparticle (NP) aggregates of commercial cholesterol oxidase (ChOx) were prepared by desolvation method. The formation and characterization of ChOxNP aggregates were studied by transmission electron microscopy and scanning electron microscopy. NP aggregates were more stable, active and had a higher shelf life than that of free enzyme. An amperometric cholesterol biosensor was constructed by immobilizing ChOxNPs onto Au electrode. The biosensor showed optimum response within 8 s at pH 6.0 and 35 Degree-Sign C, when polarized at +0.27 V versus Ag/AgCl. The biosensor possesses high sensitivity and measures cholesterol concentrations as low as 1.56 mg/dl. The working linear range was 12.5-700 mg/dl for cholesterol. The biosensor was evaluated and employed for measurement of total cholesterol in human serum. The enzyme electrode lost 50 % of its initial activity during its regular use for 180 times over a period of 90 days when stored in 0.1 M sodium phosphate buffer, pH 7.0 at 4 Degree-Sign C.

  17. Simultaneous Voltammetric/Amperometric Determination of Sulfide and Nitrite in Water at BDD Electrode

    Directory of Open Access Journals (Sweden)

    Anamaria Baciu

    2015-06-01

    Full Text Available This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix.

  18. Separation and determination of flavonoids in three traditional chinese medicines by capillary electrophoresis with amperometric detection.

    Science.gov (United States)

    Wang, Wei; Lin, Ping; Ma, Lihong; Xu, Kaixuan; Lin, Xiuli

    2016-04-01

    Flavonoids are important active ingredients in many traditional Chinese medicines. In this paper, capillary electrophoresis with amperometric detection was employed to separate and detect eight flavonoids, rutin, quercetrin, quercetin, kaempferol, kaempferide, catechin, apigenin, and luteolin, in a home-made capillary electrophoresis device. Under the separation voltage of 2000 V, the eight flavonoids could be completely separated within 33 min in 18 mM borax running buffer at pH 10.2. Good linear relationships were obtained for all analytes and the detection limits for flavonoids ranged from 0.46 to 0.85 μM. Then, the method was applied to separate and determine the flavonoids in three traditional Chinese medicines, hippophae rhamnoides, hypericum perforatum, and cacumen platycladi. Finally, rutin, kaempferol, quercetin, and quercetrin were discovered in these medicines and the concentrations ranged from 0.28 to 9.94 mg/g. The recoveries of flavonoids ranged from 84.7 to 113%, which showed the high reliability of this method. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. [Properties of modified amperometric biosensors based on methanol dehydrogenase and Methylobacterium nodulans cells].

    Science.gov (United States)

    Kuznetsova, T A; Beschastnyĭ, A P; Alferov, S V; Trotsenko, Iu A

    2013-01-01

    The properties of amperometric biosensors based on methanol dehydrogenase (MDH), Methylobacterium nodulans cells, and the ferrocene-modified carbon paste electrode were investigated. It was shown that the addition ofhydroxyapatite (HA) to a carbon paste increased the sensitivity and operating stability of MDH biosensors. The linear range of the electrode was 0.0135-0.5 and 0.032-1.5 mM for methanol and formaldehyde, respectively. The detection limit of methanol and formaldehyde was 4.5 and 11.0 microM, respectively. The loss of activity of the electrode within 10 days of storage in the presence of 2.0 mM KCN did not exceed 12%. Cyanide (10 mM) completely inhibited the sensor responses to formaldehyde (1.0 mM), which allowed for the selective determination of methanol in the presence of formaldehyde. The biosensor based on cells exhibited lower stability and sensitivity toward methanol and formaldehyde; the sensitivity coefficients were 980 and 21 nA/mM, respectively.

  20. Amperometric Enzyme-based Gas Sensor for Formaldehyde: Impact of Possible Interferences

    Directory of Open Access Journals (Sweden)

    Ralf Moos

    2007-02-01

    Full Text Available In this work, cross-sensitivities and environmental influences on the sensitivityand the functionality of an enzyme-based amperometric sensor system for the directdetection of formaldehyde from the gas phase are studied. The sensor shows a linearresponse curve for formaldehyde in the tested range (0 - 15 vppm with a sensitivity of1.9 μA/ppm and a detection limit of about 130 ppb. Cross-sensitivities by environmentalgases like CO2, CO, NO, H2, and vapors of organic solvents like methanol and ethanol areevaluated as well as temperature and humidity influences on the sensor system. The sensorshowed neither significant signal to CO, H2, methanol or ethanol nor to variations in thehumidity of the test gas. As expected, temperature variations had the biggest influence onthe sensor sensitivity with variations in the sensor signal of up to 10 % of the signal for 5vppm CH2O in the range of 25 - 30 °C.

  1. Microchip electrophoresis with amperometric detection for a novel determination of phenolic compounds in olive oil.

    Science.gov (United States)

    Godoy-Caballero, María del Pilar; Acedo-Valenzuela, María Isabel; Galeano-Díaz, Teresa; Costa-García, Agustín; Fernández-Abedul, María Teresa

    2012-11-07

    The relevance of the development of microchip electrophoresis applications in the field of food analysis is considered in this work. A novel method to determine important phenolic compounds in extra virgin olive oil samples using a miniaturized chemical analysis system is presented in this paper. Three interesting phenolic compounds in olive oil and fruit (tyrosol, hydroxytyrosol and oleuropein glucoside) were studied by end-channel amperometric detection using a 100 μm gold wire as working electrode in glass microchip electrophoresis. The electrochemical behavior of these compounds was studied and the medium to carry out their detection was selected (0.1 M aqueous sulfuric acid). The best conditions for the separation were achieved in sodium tetraborate (10% methanol, pH 9.50) with different concentrations for the sample and the running buffer in order to allow the sample stacking phenomenon. The injection was carried out using 600 V for 3 s and the separation voltage was set at 1000 V. The quality of the method was evaluated through its analytical figures of merit and by its performance on real extra virgin olive oil samples. Determination of these compounds was carried out using the standard addition calibration method with good recoveries.

  2. Amperometric detection of hydrazine utilizing synergistic action of prussian blue @ silver nanoparticles / graphite felt modified electrode

    International Nuclear Information System (INIS)

    Zhao, Jihua; Liu, Jianxin; Tricard, Simon; Wang, Lei; Liang, Yanling; Cao, Linghua; Fang, Jian; Shen, Weiguo

    2015-01-01

    Highlights: • Prussian Blue (PB) deposition on Ag/GF for electrochemical hydrazine sensing; • Lower detection limit of 4.9 × 10 −7 mol L −1 , stable over 24 days; • High sensitivity: 26.06 A mol −1 L. -- Abstract: In this study, a triple-component hydrazine sensor (PB@Ag/GF) was fabricated with freestanding graphite felt (GF), silver nanoparticles (Ag) and prussian blue (PB). The Ag nanoparticles were electrodeposited on GF ultrasonically (Ag/GF), and acted as a catalyst of the chemical deposition of PB. The electrode was characterized by scanning election microscopy (SEM), infrared spectroscopy (IR), X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDS). The electrochemical behavior of PB@Ag/GF was measured by cyclic voltammetry and amperometric measurements. The sensor displayed a prominent electrocatalytic activity toward hydrazine oxidation, with a fast response time of 2 s, a low detection limit of 4.9 × 10 −7 mol L −1 and very high detection sensitivity of 26.06 A mol −1 L

  3. Determination of plutonium and neptunium in various materials by coulometric titration with amperometric indicating

    International Nuclear Information System (INIS)

    Moiseev, I.V.; Kuperman, A.Ya.; Borodina, N.N.; Galkina, V.N.; Nikitskaya, V.N.

    1976-01-01

    Coulometric methods of determining Pu and Np in the products of complex composition containing, in addition to Pu and Np, Cr and Nn have been developed. The methods are based on titration of Pusup((6)) and Npsup((6)) to tetravalent state in H 2 SO 4 -H 3 PO 4 with iron (2) ions generated continuously. A new variant of amperometric method has been proposed for determining end-point of titration. The methods of preparing Pusup((6)) and Npsup((6)) solutions have been developed. It has been shown that, upon dissolution of PuO 2 and NpO 2 by boiling with a mixture of nitric and perchloric acids Pusup((4)) and Npsup((4)) are oxidized quantitatively to Pusup((6)) and Npsup((6)) while Cl 2 , Crsup((6)) and Mnsup((7,4,3)) in the solution obtained are selectively reduced by CHOOH and CH 2 (COOH) 2 . In 6-8 M in terms of H 2 SO 4 solution, ammonium bichromate oxidizes Npsup((4)) to Npsup((6)), Pusup((3)) to Pusup((4)), and Mnsup((2)) to Mnsup((3)). Oxidized Mn and excess of Crsup((6)) are selectively reduced by CHOOH and H 2 C 2 O 4 in 4M in terms of H 2 SO 4 solution

  4. Amperometric Acetylcholinesterase Biosensor Based on Multilayer Multiwall Carbon Nanotubes-chitosan Composite

    Directory of Open Access Journals (Sweden)

    Xia SUN

    2011-11-01

    Full Text Available A simple method for immobilization of acetylcholinesterase (AChE onto the glassy carbon electrode (GCE modified with five layers of multiwall carbon nanotubes (MWNTs-chitosan (CHIT composite was proposed, and thus a fast, sensitive and stable amperometric sensor for quantitative determination of pesticides was developed. Five layers of MWNTs-CHIT promoted electron transfer reactions at a lower potential and catalyzed the electro-oxidation of thiocholine, thus, it improved the detection sensitivity of biosensor. Based on the inhibition of pesticides to the enzymatic activity of AChE, using carbofuran as a model compound, under optimal conditions, the inhibition of carbofuran was proportional to its concentration in two ranges, from 5×10-4 to 7.5 μg/mL and 7.5 to 20 μg/mL with a detection limit of 1×10-4 μg/mL. The constructed biosensor showed prominent characteristics and performances such as good precision, acceptable stability, fast response and low detection limit, which provided a new promising tool for pesticide analysis.

  5. Preparation of cholesterol oxidase nanoparticles and their application in amperometric determination of cholesterol

    International Nuclear Information System (INIS)

    Chawla, Sheetal; Rawal, Rachna; Sonia; Ramrati; Pundir, C. S.

    2013-01-01

    The nanoparticle (NP) aggregates of commercial cholesterol oxidase (ChOx) were prepared by desolvation method. The formation and characterization of ChOxNP aggregates were studied by transmission electron microscopy and scanning electron microscopy. NP aggregates were more stable, active and had a higher shelf life than that of free enzyme. An amperometric cholesterol biosensor was constructed by immobilizing ChOxNPs onto Au electrode. The biosensor showed optimum response within 8 s at pH 6.0 and 35 °C, when polarized at +0.27 V versus Ag/AgCl. The biosensor possesses high sensitivity and measures cholesterol concentrations as low as 1.56 mg/dl. The working linear range was 12.5–700 mg/dl for cholesterol. The biosensor was evaluated and employed for measurement of total cholesterol in human serum. The enzyme electrode lost 50 % of its initial activity during its regular use for 180 times over a period of 90 days when stored in 0.1 M sodium phosphate buffer, pH 7.0 at 4 °C

  6. Detection of Benzoic Acid by an Amperometric Inhibitor Biosensor Based on Mushroom Tissue Homogenate

    Directory of Open Access Journals (Sweden)

    Mustafa Kemal Sezgintürk

    2005-01-01

    Full Text Available An amperometric benzoic acid-sensing inhibitor biosensor was prepared by immobilizing mushroom (Agaricus bisporus tissue homogenate on a Clark-type oxygen electrode. The effects of the quantity of mushroom tissue homogenate, the quantity of gelatin and the effect of the crosslinking agent glutaraldehyde percent on the biosensor were studied. The optimum concentration of phenol used as substrate was 200 μM. The bioanalytical properties of the proposed biosensor, such as dependence of the biosensor response on the pH value and the temperature, were investigated. The biosensor responded linearly to benzoic acid in a concentration range of 25–100 μM. Standard deviation (s.d. was ±0.49 μM for 7 successive determinations at a concentration of 75 μM. The inhibitor biosensor based on mushroom tissue homogenate was applied for the determination of benzoic acid in fizzy lemonade, some fruits and groundwater samples. Results were compared to those obtained using AOAC method, showing a good agreement.

  7. Characterisation of brewpub beer carbohydrates using high performance anion exchange chromatography coupled with pulsed amperometric detection.

    Science.gov (United States)

    Arfelli, Giuseppe; Sartini, Elisa

    2014-01-01

    High performance anion exchange chromatography (HPAEC) coupled with pulsed amperometric detection (PAD) was optimised in order to quantify mannose, maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose and maltoheptaose content of beer. The method allows the determination of above mentioned oligosaccharides, in a single chromatographic run, without any pre-treatment. Limit of detection and limit of quantification were suitable for beer. Accuracy and repeatability were good for the entire amount considered. Once optimised HPAEC PAD for the specific matrix, the second goal of this research was to verify the possibility to discriminate beers, depending on their style. The carbohydrates content of brewpub commercial beers was very variable, ranging from 19.3 to 1469mg/L (mannose), 34.5 to 2882mg/L (maltose), 141.9 to 20731mg/L (maltotriose), 168.5 to 7650mg/L (maltotetraose), 20.1 to 2537mg/L (maltopentaose), 22.9 to 3295mg/L (maltohexaose), 8.5 to 2492mg/L (maltoeptaose), even in the same style of beer. However, the carbohydrates content was useful, jointed with other compounds amount, to discriminate different styles of beer. As a matter of fact, principal component analysis put in evidence beer differences considering some fermentation conditions and colour. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Amperometric Formaldehyde Sensor Based on a Pd Nanocrystal Modified C/Co2P Electrode

    Directory of Open Access Journals (Sweden)

    Huan Wang

    2017-01-01

    Full Text Available Ultrafine Pd nanocrystals were grown on the cobalt phosphide (Co2P decorated Vulcan XC-72 carbon (C/Co2P, which is realized by first implementing the corresponding metal precursor and then the further chemical reduction process. The as-synthesized C/Co2P/Pd composite was further constructed to form a gas permeable electrode. This electrode can be applied for formaldehyde (HCHO detection. The results demonstrate that the Co2P nanocrystal can significantly improve the sensing performance of the C/Co2P/Pd electrode for catalytic oxidation of HCHO, which is considered to be attributed to the effective electron transfer from Co2P to Pd in the C/Co2P/Pd composites. Furthermore, the assembled C/Co2P/Pd sensor exhibits high sensitivity of 617 nA/ppm and good selectivity toward various interfering gases such as NO2, NO, SO2, CO2, and CO. It also shows the excellent linear response that the correlation coefficient is 0.994 in the concentration range of 1–10 ppm. Therefore, the proposed cost-effective C/Co2P/Pd nanocomposite, which owns advantages such as high activity and good stability, has the potential to be applied as an effective electrocatalyst for amperometric HCHO detection.

  9. Amperometric Determination of Sulfite by Gas Diffusion- Sequential Injection with Boron-Doped Diamond Electrode

    Directory of Open Access Journals (Sweden)

    Orawon Chailapakul

    2008-03-01

    Full Text Available A gas diffusion sequential injection system with amperometric detection using aboron-doped diamond electrode was developed for the determination of sulfite. A gasdiffusion unit (GDU was used to prevent interference from sample matrices for theelectrochemical measurement. The sample was mixed with an acid solution to generategaseous sulfur dioxide prior to its passage through the donor channel of the GDU. Thesulfur dioxide diffused through the PTFE hydrophobic membrane into a carrier solution of 0.1 M phosphate buffer (pH 8/0.1% sodium dodecyl sulfate in the acceptor channel of theGDU and turned to sulfite. Then the sulfite was carried to the electrochemical flow cell anddetected directly by amperometry using the boron-doped diamond electrode at 0.95 V(versus Ag/AgCl. Sodium dodecyl sulfate was added to the carrier solution to preventelectrode fouling. This method was applicable in the concentration range of 0.2-20 mgSO32−/L and a detection limit (S/N = 3 of 0.05 mg SO32−/L was achieved. This method wassuccessfully applied to the determination of sulfite in wines and the analytical resultsagreed well with those obtained by iodimetric titration. The relative standard deviations forthe analysis of sulfite in wines were in the range of 1.0-4.1 %. The sampling frequency was65 h−1.

  10. Amperometric Self-Referencing Ceramic Based Microelectrode Arrays for D-Serine Detection.

    Science.gov (United States)

    Campos-Beltrán, Diana; Konradsson-Geuken, Åsa; Quintero, Jorge E; Marshall, Lisa

    2018-03-06

    D-serine is the major D-amino acid in the mammalian central nervous system. As the dominant co-agonist of the endogenous synaptic NMDA receptor, D-serine plays a role in synaptic plasticity, learning, and memory. Alterations in D-serine are linked to neuropsychiatric disorders including schizophrenia. Thus, it is of increasing interest to monitor the concentration of D-serine in vivo as a relevant player in dynamic neuron-glia network activity. Here we present a procedure for amperometric detection of D-serine with self-referencing ceramic-based microelectrode arrays (MEAs) coated with D-amino acid oxidase from the yeast Rhodotorula gracilis (RgDAAO). We demonstrate in vitro D-serine recordings with a mean sensitivity of 8.61 ± 0.83 pA/µM to D-serine, a limit of detection (LOD) of 0.17 ± 0.01 µM, and a selectivity ratio of 80:1 or greater for D-serine over ascorbic acid (mean ± SEM; n = 12) that can be used for freely moving studies.

  11. Determination of Different Saccharides Concentration by Means of a Multienzymes Amperometric Biosensor

    Directory of Open Access Journals (Sweden)

    Marianna Portaccio

    2017-01-01

    Full Text Available A three-electrode amperometric biosensor for the detection of two different saccharides (lactose and glucose in aqueous solutions is described. On the graphite working electrode, the glucose oxidase (GOD and β-galactosidase (β-gal were coimmobilized by means of covalent bonding. The response of the biosensor as a function of the relative concentration of the two immobilized enzymes was investigated and the best working conditions were identified by measuring the sensitivity and the linear range response. In particular, our best lactose biosensor shows a linear range up to 0.010 mM and a limit of detection (LOD and a sensitivity equal to 0.001 mM and 850 ± 81 μA/mM, respectively. For glucose, the values of the above-mentioned parameters are equal to 0.015 mM for the linear range, 0.001 mM for LOD, and 505 ± 55 μA/mM for the sensitivity. The working parameters of our biosensors are significant in comparison with other biosensors developed for concentration determination of the two saccharides investigated in the present work. In particular, low (LOD and high sensitivities are obtained for lactose and glucose. To challenge our biosensor with real samples, it was tested using fruit juices, skim milk, and whey.

  12. Amperometric biosensor based on a single antibody of dual function for rapid detection of Streptococcus agalactiae.

    Science.gov (United States)

    Vásquez, Gersson; Rey, Alba; Rivera, Camilo; Iregui, Carlos; Orozco, Jahir

    2017-01-15

    Pathogenic bacteria are responsible for several diseases in humans and in a variety of hosts. Detection of pathogenic bacteria is imperative to avoid and/or fight their potential harmful effects. This work reports on the first amperometric biosensor for the rapid detection of Streptococcus agalactiae (S. agalactiae). The biosensor relies on a single biotinylated antibody that immobilizes the bacteria on a screen-printed carbon electrode while is further linked to a streptavidin-conjugated HRP reporter. The biotinylated antibody provides selectivity to the biosensor whereas serves as an anchoring point to the reporter for further amplification of the electrochemical signal. The resultant immunosensor is simple, responds rapidly, and allows for the selective and highly sensitive quantification of S. agalactiae cells in a concentration range of 10 1 -10 7 CFUml -1 , with a detection limit of 10CFUml -1 . The approach not only enables a rapid detection and quantification of S. agalactiae in environmental samples but also opens up new opportunities for the simple fabrication of electrochemical immunosensors for different target pathogens. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Improvement of Amperometric Sensor Used for Determination of Nitrate with Polypyrrole Nanowires Modified Electrode

    Directory of Open Access Journals (Sweden)

    Shi-chang Wang

    2005-12-01

    Full Text Available Polypyrrole(PPy nanowire modified electrodes were developed by template-freeelectrochemical method based on graphite electrode. The modified electrode wascharacterized by their amperometric response towards nitrate ions. Before reduction ofnitrate ions, electrochemical solid-phase extraction (EC-SPE of nitrate in/on modifiedelectrodes was conducted. It is found that the unusual nanowired structure of polypyrrolelayer (instead of well known cauliflower structure allows us to increase the effectivesurface area of the electrode and subsequently the sensitivity. And the effects ofelectrochemical preparation parameters of PPy nanowire modified electrodes on theircorresponding characters were evaluated. The experimental results show that theelectrochemical preparation parameters of the modified electrodes such as scan rate,polymerization potential, temperature of polymerization solution and polymerization timehave significantly effects on the morphology of PPy nanowires and subsequently effectivesurface area of the electrode and electroreduction current density of nitrate. Thedetermination sensitivity may be varied according to the modification parameters. Under acertain polymerization conditions, the corresponding sensitivity reaches 336.28 mA/M cm2 and the detection limit is 1.52×10-6 M. The proposed method was successfully applied in thedetection of nitrate in the real samples.

  14. Amperometric Immunosensor Based on a Protein A/Deposited Gold Nanocrystals Modified Electrode for Carbofuran Detection

    Directory of Open Access Journals (Sweden)

    Xia Sun

    2011-12-01

    Full Text Available In this paper, an amperometric immunosensor modified with protein A/deposited gold nanocrystals (DpAu was developed for the ultrasensitive detection of carbofuran residues. First, DpAu were electrodeposited onto the Au electrode surface to absorb protein A (PA and improve the electrode conductivity. Then PA was dropped onto the surface of DpAu film, used for binding antibody Fc fragments. Next, anti-carbofuran monoclonal antibody was immobilized on the PA modified electrode. Finally, bovine serum albumin (BSA was employed to block the possible remaining active sites avoiding any nonspecific adsorption. The fabrication procedure of the immunosensor was characterized by electrochemical impedance spectroscopy (EIS and cyclic voltammetry (CV, respectively. With the excellent electroconductivity of DpAu and the PA’s oriented immobilization of antibodies, a highly efficient immuno-reaction and detection sensitivity could be achieved. The influences of the electrodeposition time of DpAu, pH of the detection solution and incubation time on the current response of the fabricated immunosensor were investigated. Under optimized conditions, the current response was proportional to the concentration of carbofuran which ranged from 1 to 100 ng/mL and 100 ng/mL to 100 μg/mL. The detection limit was 0.1924 ng/mL. The proposed carbofuran immnuosensor exhibited high specificity, reproducibility, stability and regeneration performance, which may open a new door for ultrasensitive detection of carbofuran residues in vegetables and fruits.

  15. Electrooxidation and amperometric determination of vorinostat on hierarchical leaf-like gold nanolayers.

    Science.gov (United States)

    Vais, R Dehdari; Karimian, K; Heli, H

    2018-02-01

    Hierarchical leaf-like gold nanolayers were electrodeposited using choline chloride as a shape directing agent and characterized using field emission scanning electron microscopy. The electrooxidation behavior of vorinostat was then studied on the nanolayers and the kinetic parameters of the electrodic process were obtained by voltammetric measurements in a phosphate buffer solution at pH 7.40. Vorinostat was electrooxidized on the nanolayers' surface at a lower potential and with a higher rate, compared to a polycrystalline smooth gold surface, through an irreversible process. Based on the results, an amperometric sensor was designed using the hierarchical leaf-like gold nanolayers for the determination of vorinostat. A linear dynamic range of 4.0-52μmol L -1 with a calibration sensitivity of 7.7mAmol -1 L, and a detection limit of 1.40μmolL -1 were obtained. The amperometry method was also applied to the analysis of vorinostat capsules. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. A matched-filter algorithm to detect amperometric spikes resulting from quantal secretion.

    Science.gov (United States)

    Balaji Ramachandran, Supriya; Gillis, Kevin D

    2018-01-01

    Electrochemical microelectrodes located immediately adjacent to the cell surface can detect spikes of amperometric current during exocytosis as the transmitter released from a single vesicle is oxidized on the electrode surface. Automated techniques to detect spikes are needed in order to quantify the spike rate as a measure of the rate of exocytosis. We have developed a Matched Filter (MF) detection algorithm that scans the data set with a library of prototype spike templates while performing a least-squares fit to determine the amplitude and standard error. The ratio of the fit amplitude to the standard error constitutes a criterion score that is assigned for each time point and for each template. A spike is detected when the criterion score exceeds a threshold and the highest-scoring template and the time of peak score is identified. The search for the next spike commences only after the score falls below a second, lower threshold to reduce false positives. The approach was extended to detect spikes with double-exponential decays with the sum of two templates. Receiver Operating Characteristic plots (ROCs) demonstrate that the algorithm detects >95% of manually identified spikes with a false-positive rate of ∼2%. ROCs demonstrate that the MF algorithm performs better than algorithms that detect spikes based on a derivative-threshold approach. The MF approach performs well and leads into approaches to identify spike parameters. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Double electrochemical covalent coupling method based on click chemistry and diazonium chemistry for the fabrication of sensitive amperometric immunosensor.

    Science.gov (United States)

    Qi, Honglan; Li, Min; Zhang, Rui; Dong, Manman; Ling, Chen

    2013-08-20

    A double electrochemical covalent coupling method based on click chemistry and diazonium chemistry for the fabrication of sensitive amperometric immunosensor was developed. As a proof-of-concept, a designed alkyne functionalized human IgG was used as a capture antibody and a HRP-labeled rabbit anti-goat IgG was used as signal antibody for the determination of the anti-human IgG using the sandwich model. The immunosensor was fabricated by electrochemically grafting a phenylazide on the surface of a glassy carbon electrode, and then, by coupling the alkyne functionalized human IgG with the phenylazide group through an electro-click chemistry in the presence of Cu(II). The amperometric measurement for the determination of the anti-human IgG was performed after the fabricated immunosensor was incubated with the target anti-human IgG and then with the HRP-labeled anti-goat IgG at -0.25V in 0.10M PBS (pH 7.0) containing 0.1mM hydroquinone and 2.0mM H2O2. The results showed that the increased current was linear with the logarithm of the concentration of the anti-human IgG in the range from 1.0×10(-10)g mL(-1) to 1.0×10(-8)g mL(-1) with a detection limit of 3×10(-11)g mL(-1). Furthermore, the feasibility of the double electrochemical covalent coupling method proposed in this work for fabricating the amperometric immunosensor array was explored. This work demonstrates that the double electrochemical covalent coupling method is a promising approach for the fabrication of the immunosensor and immunosensor array. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Simple approach for the fabrication of screen-printed carbon-based electrode for amperometric detection on microchip electrophoresis.

    Science.gov (United States)

    Petroni, Jacqueline Marques; Lucca, Bruno Gabriel; Ferreira, Valdir Souza

    2017-02-15

    This paper describes a simple method for the fabrication of screen-printed based electrodes for amperometric detection on microchip electrophoresis (ME) devices. The procedure developed is quite simple and does not require expensive instrumentation or sophisticated protocols commonly employed on the production of amperometric sensors, such as photolithography or sputtering steps. The electrodes were fabricated through manual deposition of home-made conductive carbon ink over patterned acrylic substrate. Morphological structure and electrochemical behavior of the carbon electrodes were investigated by scanning electron microscopy and cyclic voltammetry. The produced amperometric sensors were coupled to polydimethylsiloxane (PDMS) microchips at end-channel configuration in order to evaluate their analytical performance. For this purpose, electrophoretic experiments were carried out using nitrite and ascorbic acid as model analytes. Separation of these substances was successfully performed within 50s with good resolution (R = 1.2) and sensitivities (713.5 pA/μM for nitrite and 255.4 pA/μM for ascorbate). The reproducibility of the fabrication method was evaluated and revealed good values concerning the peak currents obtained (8.7% for nitrite and 9.3% for ascorbate). The electrodes obtained through this method exhibited satisfactory lifetime (ca. 400 runs) over low fabrication cost (less than $1 per piece). The feasibility of the proposed device for real analysis was demonstrated through the determination of nitrite concentration levels in drinking water samples. Based on the results achieved, the approach proposed here shows itself as an interesting alternative for simple fabrication of carbon-based electrodes. Furthermore, the devices indicate great promise for other kind of analytical applications involving ME devices. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Critical Evaluation of Acetylcholine Determination in Rat Brain Microdialysates using Ion-Pair Liquid Chromatography with Amperometric Detection

    Directory of Open Access Journals (Sweden)

    Yvette Michotte

    2008-08-01

    Full Text Available Liquid chromatography with amperometric detection remains the most widely used method for acetylcholine quantification in microdialysis samples. Separation of acetylcholine from choline and other matrix components on a microbore chromatographic column (1 mm internal diameter, conversion of acetylcholine in an immobilized enzyme reactor and detection of the produced hydrogen peroxide on a horseradish peroxidase redox polymer coated glassy carbon electrode, achieves sufficient sensitivity for acetylcholine quantification in rat brain microdialysates. However, a thourough validation within the concentration range required for this application has not been carried out before. Furthermore, a rapid degradation of the chromatographic columns and enzyme systems have been reported. In the present study an ion-pair liquid chromatography assay with amperometric detection was validated and its long-term stability evaluated. Working at pH 6.5 dramatically increased chromatographic stability without a loss in sensitivity compared to higher pH values. The lower limit of quantification of the method was 0.3 nM. At this concentration the repeatability was 15.7%, the inter-day precision 8.7% and the accuracy 103.6%. The chromatographic column was stable over 4 months, the immobilized enzyme reactor up to 2-3 months and the enzyme coating of the amperometric detector up to 1-2 months. The concentration of acetylcholine in 30 μl microdialysates obtained under basal conditions from the hippocampus of freely moving rats was 0.40 ± 0.12 nM (mean ± SD, n = 30. The present method is therefore suitable for acetylcholine determination in rat brain microdialysates.

  20. Development of an Amperometric Biosensor Platform for the Combined Determination of L-Malic, Fumaric, and L-Aspartic Acid.

    Science.gov (United States)

    Röhlen, Désirée L; Pilas, Johanna; Schöning, Michael J; Selmer, Thorsten

    2017-10-01

    Three amperometric biosensors have been developed for the detection of L-malic acid, fumaric acid, and L -aspartic acid, all based on the combination of a malate-specific dehydrogenase (MDH, EC 1.1.1.37) and diaphorase (DIA, EC 1.8.1.4). The stepwise expansion of the malate platform with the enzymes fumarate hydratase (FH, EC 4.2.1.2) and aspartate ammonia-lyase (ASPA, EC 4.3.1.1) resulted in multi-enzyme reaction cascades and, thus, augmentation of the substrate spectrum of the sensors. Electrochemical measurements were carried out in presence of the cofactor β-nicotinamide adenine dinucleotide (NAD + ) and the redox mediator hexacyanoferrate (III) (HCFIII). The amperometric detection is mediated by oxidation of hexacyanoferrate (II) (HCFII) at an applied potential of + 0.3 V vs. Ag/AgCl. For each biosensor, optimum working conditions were defined by adjustment of cofactor concentrations, buffer pH, and immobilization procedure. Under these improved conditions, amperometric responses were linear up to 3.0 mM for L-malate and fumarate, respectively, with a corresponding sensitivity of 0.7 μA mM -1 (L-malate biosensor) and 0.4 μA mM -1 (fumarate biosensor). The L-aspartate detection system displayed a linear range of 1.0-10.0 mM with a sensitivity of 0.09 μA mM -1 . The sensor characteristics suggest that the developed platform provides a promising method for the detection and differentiation of the three substrates.

  1. An amperometric biosensor for glucose detection from glucose oxidase immobilized in polyaniline-polyvinylsulfonate-potassium ferricyanide film.

    Science.gov (United States)

    Arslan, Fatma; Beskan, Umut

    2014-08-01

    In this study, a novel amperometric glucose biosensor with immobilization of glucose oxidase on electrochemically polymerized polyaniline-polyvinylsulphonate-potassium ferricyanide (Pani-Pvs-Fc) films has been accomplished via the entrapment technique. Potassium ferricyanide was used as the mediator. Determination of glucose was carried out by the oxidation of potassium ferrocyanide at 0.3 V vs. Ag/AgCl. The effects of pH and temperature were investigated, and the optimum pH value was found to be 7.5. The storage stability and the operational stability of the enzyme electrode were also studied.

  2. Simple approach for the fabrication of screen-printed carbon-based electrode for amperometric detection on microchip electrophoresis

    International Nuclear Information System (INIS)

    Petroni, Jacqueline Marques; Lucca, Bruno Gabriel; Ferreira, Valdir Souza

    2017-01-01

    This paper describes a simple method for the fabrication of screen-printed based electrodes for amperometric detection on microchip electrophoresis (ME) devices. The procedure developed is quite simple and does not require expensive instrumentation or sophisticated protocols commonly employed on the production of amperometric sensors, such as photolithography or sputtering steps. The electrodes were fabricated through manual deposition of home-made conductive carbon ink over patterned acrylic substrate. Morphological structure and electrochemical behavior of the carbon electrodes were investigated by scanning electron microscopy and cyclic voltammetry. The produced amperometric sensors were coupled to polydimethylsiloxane (PDMS) microchips at end-channel configuration in order to evaluate their analytical performance. For this purpose, electrophoretic experiments were carried out using nitrite and ascorbic acid as model analytes. Separation of these substances was successfully performed within 50s with good resolution (R = 1.2) and sensitivities (713.5 pA/μM for nitrite and 255.4 pA/μM for ascorbate). The reproducibility of the fabrication method was evaluated and revealed good values concerning the peak currents obtained (8.7% for nitrite and 9.3% for ascorbate). The electrodes obtained through this method exhibited satisfactory lifetime (ca. 400 runs) over low fabrication cost (less than $1 per piece). The feasibility of the proposed device for real analysis was demonstrated through the determination of nitrite concentration levels in drinking water samples. Based on the results achieved, the approach proposed here shows itself as an interesting alternative for simple fabrication of carbon-based electrodes. Furthermore, the devices indicate great promise for other kind of analytical applications involving ME devices. - Highlights: • A novel method to fabricate screen-printed electrodes for amperometric detection in ME is demonstrated. • No sophisticated

  3. Analysis of human milk oligosaccharides using high-performance anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    ) and lacto-N-neotetraose (Galβ1-4GlcNAcβ1-3Galβ1-4Glc), among others. High-performance anion-exchange chromatography (HPAE) with pulsed amperometric detection (PAD) is an analysis method highly suited for carbohydrates. HPAE with alkaline eluents results in retention of neutral carbohydrates depending...... on the number of charged group in the molecule, pH and concentration of competing anions, while the PAD has sensitivity for carbohydrates in the pmol-range (Lee 1990). As a basis for the development and optimisation of HPAE elution methods, the parameter space was investigated in terms of eluent concentrations...

  4. Separation of human milk oligosaccharides using high-performance anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Lie, Aleksander; Pedersen, Lars Haastrup

    individual mothers is considerable, ranging from as few as 23 and up to 130 different oligosaccharides. HMOs are known as beneficial for infant health and development, and have received increasing attention in recent years (Bode & Jantscher-Krenn 2012). High-performance anion-exchange chromatography (HPAE......) with pulsed amperometric detection (PAD) is an analysis method highly suited for carbohydrates. HPAE with alkaline eluents results in retention of neutral carbohydrates depending on the number of charged groups in the molecule, pH and concentration of competing anions, while PAD has sensitivity...

  5. Simple approach for the fabrication of screen-printed carbon-based electrode for amperometric detection on microchip electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Petroni, Jacqueline Marques [Instituto de Química, Universidade Federal de Mato Grosso do Sul, Campo Grande, MS, 79074-460 (Brazil); Lucca, Bruno Gabriel, E-mail: bruno.lucca@ufes.br [Departamento de Ciências Naturais, Universidade Federal do Espírito Santo, São Mateus, ES, 29932-540 (Brazil); Ferreira, Valdir Souza [Instituto de Química, Universidade Federal de Mato Grosso do Sul, Campo Grande, MS, 79074-460 (Brazil)

    2017-02-15

    This paper describes a simple method for the fabrication of screen-printed based electrodes for amperometric detection on microchip electrophoresis (ME) devices. The procedure developed is quite simple and does not require expensive instrumentation or sophisticated protocols commonly employed on the production of amperometric sensors, such as photolithography or sputtering steps. The electrodes were fabricated through manual deposition of home-made conductive carbon ink over patterned acrylic substrate. Morphological structure and electrochemical behavior of the carbon electrodes were investigated by scanning electron microscopy and cyclic voltammetry. The produced amperometric sensors were coupled to polydimethylsiloxane (PDMS) microchips at end-channel configuration in order to evaluate their analytical performance. For this purpose, electrophoretic experiments were carried out using nitrite and ascorbic acid as model analytes. Separation of these substances was successfully performed within 50s with good resolution (R = 1.2) and sensitivities (713.5 pA/μM for nitrite and 255.4 pA/μM for ascorbate). The reproducibility of the fabrication method was evaluated and revealed good values concerning the peak currents obtained (8.7% for nitrite and 9.3% for ascorbate). The electrodes obtained through this method exhibited satisfactory lifetime (ca. 400 runs) over low fabrication cost (less than $1 per piece). The feasibility of the proposed device for real analysis was demonstrated through the determination of nitrite concentration levels in drinking water samples. Based on the results achieved, the approach proposed here shows itself as an interesting alternative for simple fabrication of carbon-based electrodes. Furthermore, the devices indicate great promise for other kind of analytical applications involving ME devices. - Highlights: • A novel method to fabricate screen-printed electrodes for amperometric detection in ME is demonstrated. • No sophisticated

  6. An improved amperometric creatinine biosensor based on nanoparticles of creatininase, creatinase and sarcosine oxidase.

    Science.gov (United States)

    Kumar, Parveen; Jaiwal, Ranjana; Pundir, C S

    2017-11-15

    An improved amperometric biosensor for detection of creatinine was developed based on immobilization of nanoparticles (NPs) of creatininase (CA), creatinase (CI), and sarcosine oxidase (SOx) onto glassy carbon (GC) electrode. Transmission electron microscopy (TEM) and fourier transform infrared spectroscopy (FTIR) were employed for characterization of enzyme nanoparticles (ENPs). The GC electrode was characterized by scanning electron microscopy (SEM), cyclic voltammetry (CV) and electrochemical impedance spectra (EIS) at different stages of its amendment. The biosensor showed optimum response within 2s at pH 6.0 in 0.1 M sodium phosphate buffer and 25 °C, when operated at 1.0 V against Ag/AgCl. Biosensor exhibited wider linear range from 0.01 μM to 12 μM with a limit of detection (LOD) of 0.01 μM. The analytical recoveries of added creatinine in sera were 97.97 ± 0.1% for 0.1 mM and 98.76 ± 0.2% for 0.15 mM, within and between batch coefficients of variation (CV) were 2.06% and 3.09% respectively. A good correlation (R 2  = 0.99) was observed between sera creatinine values obtained by standard enzymic colorimetric method and the present biosensor. This biosensor measured creatinine level in sera of apparently healthy subjects and persons suffering from renal and muscular dysfunction. The ENPs electrode lost 10% of its initial activity within 240 days of its regular uses, when stored at 4 °C. Copyright © 2017 Elsevier Inc. All rights reserved.

  7. A fine pointed glucose oxidase immobilized electrode for low-invasive amperometric glucose monitoring.

    Science.gov (United States)

    Li, Jiang; Koinkar, Pankaj; Fuchiwaki, Yusuke; Yasuzawa, Mikito

    2016-12-15

    A low invasive type glucose sensor, which has a sensing region at the tip of a fine pointed electrode, was developed for continuous glucose monitoring. Platinum-iridium alloy electrode with a surface area of 0.045mm(2) was settled at the middle of pointed PEEK (Polyetheretherketone) tubing and was employed as sensing electrode. Electrodeposition of glucose oxidase in the presence of surfactant, Triton X-100, was performed for high-density enzyme immobilization followed by the electropolymerization of o-phenylenediamine for the formation of functional entrapping and permselective polymer membrane. Ag/AgCl film was coated on the surface of PEEK tubing as reference electrode. Amperometric responses of the prepared sensors to glucose were measured at a potential of 0.60V (vs. Ag/AgCl). The prepared electrode showed the sensitivity of 2.55μA/cm(2) mM with high linearity of 0.9986, within the glucose concentration range up to 21mM. The detection limit (S/N=3) was determined to be 0.11mM. The glucose sensor properties were evaluated in phosphate buffer solution and in vivo monitoring by the implantation of the sensors in rabbit, while conventional needle type sensors as a reference were used. The results showed that change in output current of the proposed sensor fluctuated similar with one in output current of the conventional needle type sensors, which was also in similar accordance with actual blood sugar level measured by commercially glucose meter. One-point calibration method was used to calibrate the sensor output current. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Amperometric L-glutamate biosensor based on bacterial cell-surface displayed glutamate dehydrogenase

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Bo [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); University of Chinese Academy of Sciences, 19A Yuquan Road, Beijing 100049 (China); Zhang, Shu [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, 238 Songling Road, Qingdao 266100 (China); Lang, Qiaolin [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); Song, Jianxia; Han, Lihui [Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, 238 Songling Road, Qingdao 266100 (China); Liu, Aihua, E-mail: liuah@qibebt.ac.cn [Laboratory for Biosensing, Key Laboratory of Biofuels, and Shandong Provinicial Key Laboratory of Energy Genetics, Qingdao Institute of Bioenergy & Bioprocess Technology, Chinese Academy of Sciences, 189 Songling Road, Qingdao 266101 (China); University of Chinese Academy of Sciences, 19A Yuquan Road, Beijing 100049 (China)

    2015-07-16

    Highlights: • E. coli surface-dispalyed Gldh exhibiting excellent enzyme activity and stability. • Sensitive amperometric biosensor for glutamate using Gldh-bacteria and MWNTs. • The glutamate biosensor exhibited high specificity and stability. - Abstract: A novel L-glutamate biosensor was fabricated using bacteria surface-displayed glutamate dehydrogenase (Gldh-bacteria). Here the cofactor NADP{sup +}-specific dependent Gldh was expressed on the surface of Escherichia coli using N-terminal region of ice nucleation protein (INP) as the anchoring motif. The cell fractionation assay and SDS-PAGE analysis indicated that the majority of INP-Gldh fusion proteins were located on the surface of cells. The biosensor was fabricated by successively casting polyethyleneimine (PEI)-dispersed multi-walled carbon nanotubes (MWNTs), Gldh-bacteria and Nafion onto the glassy carbon electrode (Nafion/Gldh-bacteria/PEI-MWNTs/GCE). The MWNTs could not only significantly lower the oxidation overpotential towards NAPDH, which was the product of NADP{sup +} involving in the oxidation of glutamate by Gldh, but also enhanced the current response. Under the optimized experimental conditions, the current–time curve of the Nafion/Gldh-bacteria/PEI-MWNTs/GCE was performed at +0.52 V (vs. SCE) by amperometry varying glutamate concentration. The current response was linear with glutamate concentration in two ranges (10 μM–1 mM and 2–10 mM). The low limit of detection was estimated to be 2 μM glutamate (S/N = 3). Moreover, the proposed biosensor is stable, specific, reproducible and simple, which can be applied to real samples detection.

  9. Nanostructured progesterone immunosensor using a tyrosinase-colloidal gold-graphite-Teflon biosensor as amperometric transducer

    Energy Technology Data Exchange (ETDEWEB)

    Carralero, Veronica [Department of Analytical Chemistry, Faculty of Chemistry, University Complutense of Madrid, 28040 Madrid (Spain); Gonzalez-Cortes, Araceli [Department of Analytical Chemistry, Faculty of Chemistry, University Complutense of Madrid, 28040 Madrid (Spain); Yanez-Sedeno, Paloma [Department of Analytical Chemistry, Faculty of Chemistry, University Complutense of Madrid, 28040 Madrid (Spain)]. E-mail: yseo@quim.ucm.es; Pingarron, Jose M. [Department of Analytical Chemistry, Faculty of Chemistry, University Complutense of Madrid, 28040 Madrid (Spain)

    2007-07-16

    A novel progesterone immunosensor using a colloidal gold-graphite-Teflon-tyrosinase composite biosensor as amperometric transducer is reported. A sequential competitive configuration between the analyte and progesterone labelled with alkaline phosphatase (AP) was used. Phenyl phosphate was employed as the AP-substrate and the enzyme reaction product, phenol, was oxidized by tyrosinase to o-quinone, which is subsequently reduced at -0.1 V at the biocomposite electrode. Variables such as the concentration of phenyl phosphate, the amount of antibody attached to the electrode surface, immersion time in a 2% BSA solution, working pH and incubation times in progesterone and AP conjugate were optimized. A linear calibration graph for progesterone was obtained between 0 and 40 ng mL{sup -1} with a slope value of -82.3 nA ng{sup -1} mL, and a detection limit of 0.43 ng mL{sup -1}. The time needed to reach the steady-state current from the addition of phenyl phosphate was 30-40 s. These analytical characteristics improve substantially those reported for other progesterone immunosensors. A lifetime of 14 days with no need to apply any regeneration procedure was also achieved. The usefulness of the immunosensor was evaluated by determining progesterone in milk samples spiked with the analyte at 5.0 and 1.5 ng mL{sup -1} concentration levels. Following a very simple procedure, involving only sample dilution, mean recoveries (n = 7) of 98 {+-} 3% and 99 {+-} 3%, respectively, were obtained.

  10. Nanostructured progesterone immunosensor using a tyrosinase-colloidal gold-graphite-Teflon biosensor as amperometric transducer

    International Nuclear Information System (INIS)

    Carralero, Veronica; Gonzalez-Cortes, Araceli; Yanez-Sedeno, Paloma; Pingarron, Jose M.

    2007-01-01

    A novel progesterone immunosensor using a colloidal gold-graphite-Teflon-tyrosinase composite biosensor as amperometric transducer is reported. A sequential competitive configuration between the analyte and progesterone labelled with alkaline phosphatase (AP) was used. Phenyl phosphate was employed as the AP-substrate and the enzyme reaction product, phenol, was oxidized by tyrosinase to o-quinone, which is subsequently reduced at -0.1 V at the biocomposite electrode. Variables such as the concentration of phenyl phosphate, the amount of antibody attached to the electrode surface, immersion time in a 2% BSA solution, working pH and incubation times in progesterone and AP conjugate were optimized. A linear calibration graph for progesterone was obtained between 0 and 40 ng mL -1 with a slope value of -82.3 nA ng -1 mL, and a detection limit of 0.43 ng mL -1 . The time needed to reach the steady-state current from the addition of phenyl phosphate was 30-40 s. These analytical characteristics improve substantially those reported for other progesterone immunosensors. A lifetime of 14 days with no need to apply any regeneration procedure was also achieved. The usefulness of the immunosensor was evaluated by determining progesterone in milk samples spiked with the analyte at 5.0 and 1.5 ng mL -1 concentration levels. Following a very simple procedure, involving only sample dilution, mean recoveries (n = 7) of 98 ± 3% and 99 ± 3%, respectively, were obtained

  11. Nonenzymatic amperometric sensor for ascorbic acid based on hollow gold/ruthenium nanoshells

    Energy Technology Data Exchange (ETDEWEB)

    Jo, Ara; Kang, Minkyung; Cha, Areum; Jang, Hye Su [Department of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750 (Korea, Republic of); Shim, Jun Ho [Department of Chemistry, Daegu University, Gyeongsan 712-714 (Korea, Republic of); Lee, Nam-Suk [National Center for Nanomaterials Technology (NCNT), Pohang University of Science and Technology (POSTECH), Pohang 790-784 (Korea, Republic of); Kim, Myung Hwa [Department of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750 (Korea, Republic of); Lee, Youngmi, E-mail: youngmilee@ewha.ac.kr [Department of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750 (Korea, Republic of); Lee, Chongmok, E-mail: cmlee@ewha.ac.kr [Department of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750 (Korea, Republic of)

    2014-03-01

    Highlights: • We synthesized hollow gold/ruthenium (hAu–Ru) nanoshells for ascorbic acid sensing. • The hAu–Ru nanoshells showed sensitivity of 426 μA mM⁻¹ cm⁻² for ascorbic acid. • Good selectivity against glucose, uric acid, dopamine, 4-acetamidophenol, and NADH. • The linear dynamic range appeared from zero to 2.0 mM (R = 0.9995). • Response time (1.6 s) and low detection limit (2.2 μM) were obtained at pH 7.40. Abstract: We report a new nonenzymatic amperometric detection of ascorbic acid (AA) using a glassy carbon (GC) disk electrode modified with hollow gold/ruthenium (hAu–Ru) nanoshells, which exhibited decent sensing characteristics. The hAu–Ru nanoshells were prepared by the incorporation of Ru on hollow gold (hAu) nanoshells from Co nanoparticle templates, which enabled AA selectivity against glucose without aid of enzyme or membrane. The structure and electrocatalytic activities of the hAu–Ru catalysts were characterized by spectroscopic and electrochemical techniques. The hAu–Ru loaded on GC electrode (hAu–Ru/GC) showed sensitivity of 426 μA mM⁻¹ cm⁻² (normalized to the GC disk area) for the linear dynamic range of <5 μM to 2 mM AA at physiological pH. The response time and detection limit were 1.6 s and 2.2 μM, respectively. Furthermore, the hAu–Ru/GC electrode displayed remarkable selectivity for ascorbic acid over all potential biological interferents, including glucose, uric acid (UA), dopamine (DA), 4-acetamidophenol (AP), and nicotinamide adenine dinucleotide (NADH), which could be especially good for biological sensing.

  12. Nonenzymatic amperometric sensor for ascorbic acid based on hollow gold/ruthenium nanoshells

    International Nuclear Information System (INIS)

    Jo, Ara; Kang, Minkyung; Cha, Areum; Jang, Hye Su; Shim, Jun Ho; Lee, Nam-Suk; Kim, Myung Hwa; Lee, Youngmi; Lee, Chongmok

    2014-01-01

    Highlights: • We synthesized hollow gold/ruthenium (hAu–Ru) nanoshells for ascorbic acid sensing. • The hAu–Ru nanoshells showed sensitivity of 426 μA mM −1 cm −2 for ascorbic acid. • Good selectivity against glucose, uric acid, dopamine, 4-acetamidophenol, and NADH. • The linear dynamic range appeared from zero to 2.0 mM (R = 0.9995). • Response time (1.6 s) and low detection limit (2.2 μM) were obtained at pH 7.40. - Abstract: We report a new nonenzymatic amperometric detection of ascorbic acid (AA) using a glassy carbon (GC) disk electrode modified with hollow gold/ruthenium (hAu–Ru) nanoshells, which exhibited decent sensing characteristics. The hAu–Ru nanoshells were prepared by the incorporation of Ru on hollow gold (hAu) nanoshells from Co nanoparticle templates, which enabled AA selectivity against glucose without aid of enzyme or membrane. The structure and electrocatalytic activities of the hAu–Ru catalysts were characterized by spectroscopic and electrochemical techniques. The hAu–Ru loaded on GC electrode (hAu–Ru/GC) showed sensitivity of 426 μA mM −1 cm −2 (normalized to the GC disk area) for the linear dynamic range of <5 μM to 2 mM AA at physiological pH. The response time and detection limit were 1.6 s and 2.2 μM, respectively. Furthermore, the hAu–Ru/GC electrode displayed remarkable selectivity for ascorbic acid over all potential biological interferents, including glucose, uric acid (UA), dopamine (DA), 4-acetamidophenol (AP), and nicotinamide adenine dinucleotide (NADH), which could be especially good for biological sensing

  13. Amperometric Metronidazole Sensor Based on the Supermolecular Recognition by Metalloporphyrin Incorporated In Carbon Paste Electrode

    Directory of Open Access Journals (Sweden)

    Ru-Qin Yu

    2003-03-01

    Full Text Available An amperometric metronidazole (MTZ sensor using a glycosylated metalloporphyrin as a recognition element, which was incorporated in a carbon paste electrode, is reported. For the preparation of a MTZ-sensitive active material, 5, 10, 15, 20-tetrakis [2-(2, 3, 4, 6-tetraacetyl-β-D-glucopyranosyl-1-O-phenyl]porphyrin (T(oglu PPH2 and its Mn(III complex MnT(o-gluPPCl were synthesized from the reaction of pyrrole with ortho-acetylglycosylated benzaldehyde by Lindsay’s method. The MnT(oglu PPCl-modified electrode showed excellent selectivity toward MTZ with respect to a number of interferents and exhibited stable response. The calibration graph obtained with the proposed sensor was linear over the range of 2.9×10-3-5.8×10-8 M/L, with a detection limit of 5.8×10-8 M/L for MTZ. Cyclic voltammetric measurements indicated that MnT(oglu PPCl included in graphite-epoxy resin matrices could efficiently mediate electron transfer from the base electrode to MTZ causing a decrease of reduction potential for MTZ detection. The sensor could be regenerated by simply polishing with an alumina paper, with an excellent reproducibility (RSD=1.6%. The experimental conditions such as pH and applied working potential were optimized. The prepared sensor is applied for the determination of MTZ in pharmaceutical preparations and the results agreed with the values obtained by the pharmacopoeia method.

  14. A novel combined thermometric and amperometric biosensor for lactose determination based on immobilised cellobiose dehydrogenase.

    Science.gov (United States)

    Yakovleva, Maria; Buzas, Orsolya; Matsumura, Hirotoshi; Samejima, Masahiro; Igarashi, Kiyohiko; Larsson, Per-Olof; Gorton, Lo; Danielsson, Bengt

    2012-01-15

    A novel method for lactose determination in milk is proposed. It is based on oxidation of lactose by cellobiose dehydrogenase (CDH) from the basidiomycete Phanerochaete chrysosporium, immobilised in an enzyme reactor. The reactor was prepared by cross-linking CDH onto aminopropyl-silanised controlled pore glass (CPG) beads using glutaraldehyde. The combined biosensor worked in flow injection analysis (FIA) mode and was developed for simultaneous monitoring of the thermometric signal associated with the enzymatic oxidation of lactose using p-benzoquinone as electron acceptor and the electrochemically generated current associated with the oxidation of the hydroquinone formed. A highly reproducible linear response for lactose was obtained between 0.05 mM and 30 mM. For a set of more than 500 samples an R.S.D. of less than 10% was achieved. The assay time was ca. 2 min per sample. The sensor was applied for the determination of lactose in dairy milk samples (milk with a fat content of 1.5% or 3% and also "lactose free" milk). No sample preparation except dilution with buffer was needed. The proposed method is rapid, suitable for repeated use and allows the possibility to compare results from two different detection methods, thus providing a built-in quality assurance. Some differences in the response observed between the methods indicate that the dual approach can be useful in mechanistic studies of redox enzymes. In addition, a dual system opens up interesting possibilities for studies of enzyme properties and mechanisms. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Disposable Amperometric Immunosensor for the Determination of Human P53 Protein in Cell Lysates Using Magnetic Micro-Carriers

    Directory of Open Access Journals (Sweden)

    María Pedrero

    2016-11-01

    Full Text Available An amperometric magnetoimmunosensor for the determination of human p53 protein is described in this work using a sandwich configuration involving the covalent immobilization of a specific capture antibody onto activated carboxylic-modified magnetic beads (HOOC-MBs and incubation of the modified MBs with a mixture of the target protein and horseradish peroxidase-labeled antibody (HRP-anti-p53. The resulting modified MBs are captured by a magnet placed under the surface of a disposable carbon screen-printed electrode (SPCE and the amperometric responses are measured at −0.20 V (vs. an Ag pseudo-reference electrode, upon addition of hydroquinone (HQ as a redox mediator and H2O2 as the enzyme substrate. The magnetoimmunosensing platform was successfully applied for the detection of p53 protein in different cell lysates without any matrix effect after a simple sample dilution. The results correlated accurately with those provided by a commercial ELISA kit, thus confirming the immunosensor as an attractive alternative for rapid and simple determination of this protein using portable and affordable instrumentation.

  16. Nafion/lead nitroprusside nanoparticles modified carbon ceramic electrode as a novel amperometric sensor for L-cysteine.

    Science.gov (United States)

    Razmi, H; Heidari, H

    2009-05-01

    This work describes the electrochemical and electrocatalytic properties of carbon ceramic electrode (CCE) modified with lead nitroprusside (PbNP) nanoparticles as a new electrocatalyst material. The structure of deposited film on the CCE was characterized by energy dispersive X-ray (EDX), Fourier transform infrared (FTIR), and scanning electron microscopy (SEM). The cyclic voltammogram (CV) of the PbNP modified CCE showed two well-defined redox couples due to [Fe(CN)5NO](3-)/[Fe(CN)5NO](2-) and Pb(IV)/Pb(II) redox reactions. The modified electrode showed electrocatalytic activity toward the oxidation of L-cysteine and was used as an amperometric sensor. Also, to reduce the fouling effect of L-cysteine and its oxidation products on the modified electrode, a thin film of Nafion was coated on the electrode surface. The sensor response was linearly changed with L-cysteine concentration in the range of 1 x 10(-6) to 6.72 x 10(-5)mol L(-1) with a detection limit (signal/noise ratio [S/N]=3) of 0.46 microM. The sensor sensitivity was 0.17 microA (microM)(-1), and some important advantages such as simple preparation, fast response, good stability, interference-free signals, antifouling properties, and reproducibility of the sensor for amperometric determination of L-cysteine were achieved.

  17. Amperometric bienzyme glucose biosensor based on carbon nanotube modified electrode with electropolymerized poly(toluidine blue O) film

    International Nuclear Information System (INIS)

    Wang Wenju; Wang Fang; Yao Yanli; Hu Shengshui; Shiu, Kwok-Keung

    2010-01-01

    The amperometric bienzyme glucose biosensor utilizing horseradish peroxidase (HRP) and glucose oxidase (GOx) immobilized in poly(toluidine blue O) (PTBO) film was constructed on multi-walled carbon nanotube (MWNT) modified glassy carbon electrode. The HRP layer could be used to analyze hydrogen peroxide with toluidine blue O (TBO) mediators, while the bienzyme system (HRP + GOx) could be utilized for glucose determination. Glucose underwent biocatalytic oxidation by GOx in the presence of oxygen to yield H 2 O 2 which was further reduced by HRP at the MWNT-modified electrode with TBO mediators. In the absence of oxygen, glucose oxidation proceeded with electron transfer between GOx and the electrode mediated by TBO moieties without H 2 O 2 production. The bienzyme electrode offered high sensitivity for amperometric determination of glucose at low potential, displaying Michaelis-Menten kinetics. The bienzyme glucose biosensor displayed linear response from 0.1 to 1.2 mM with a sensitivity of 113 mA M -1 cm -2 at an applied potential of -0.10 V in air-saturated electrolytes.

  18. Bi-enzyme L-arginine-selective amperometric biosensor based on ammonium-sensing polyaniline-modified electrode.

    Science.gov (United States)

    Stasyuk, Nataliya; Smutok, Oleh; Gayda, Galina; Vus, Bohdan; Koval'chuk, Yevgen; Gonchar, Mykhailo

    2012-01-01

    A novel L-arginine-selective amperometric bi-enzyme biosensor based on recombinant human arginase I isolated from the gene-engineered strain of methylotrophic yeast Hansenula polymorpha and commercial urease is described. The biosensing layer was placed onto a polyaniline-Nafion composite platinum electrode and covered with a calcium alginate gel. The developed sensor revealed a good selectivity to L-arginine. The sensitivity of the biosensor was 110 ± 1.3 nA/(mM mm(2)) with the apparent Michaelis-Menten constant (K(M)(app)) derived from an L-arginine (L-Arg) calibration curve of 1.27 ± 0.29 mM. A linear concentration range was observed from 0.07 to 0.6mM, a limit of detection being 0.038 mM and a response time - 10s. The developed biosensor demonstrated good storage stability. A laboratory prototype of the proposed amperometric biosensor was applied to the samples of three commercial pharmaceuticals ("Tivortin", "Cytrarginine", "Aminoplazmal 10% E") for L-Arg testing. The obtained L-Arg-content values correlated well with those declared by producers. Copyright © 2012 Elsevier B.V. All rights reserved.

  19. A novel, disposable, screen-printed amperometric biosensor for glucose in serum fabricated using a water-based carbon ink.

    Science.gov (United States)

    Crouch, Eric; Cowell, David C; Hoskins, Stephen; Pittson, Robin W; Hart, John P

    2005-11-15

    Screen-printed amperometric glucose biosensors have been fabricated using a water-based carbon ink. The enzyme glucose oxidase (GOD) and the electro-catalyst cobalt phthalocyanine were mixed with the carbon ink prior to the screen-printing process; therefore, biosensors are prepared in a one-step fabrication procedure. Optimisation of the biosensor performance was achieved by studying the effects of pH, buffer strength, and applied potential on the analytical response. Calibration studies were performed under optimum conditions, using amperometry in stirred solution, with an operating potential of +500 mV versus SCE. The sensitivity was found to be 1170 nA mM(-1), with a linear range of 0.025-2 mM; the former represents the detection limit. The disposable amperometric biosensor was evaluated by carrying out replicate determinations on a sample of bovine serum. This was achieved by the method of multiple standard additions and included a correction for background currents arising from oxidizable serum components. The mean serum concentration was calculated to be 8.63 mM and compared well with the supplier's value of 8.3 mM; the coefficient of variation was calculated to be 3.3% (n=6).

  20. Improved in vivo performance of amperometric oxygen (PO2) sensing catheters via electrochemical nitric oxide generation/release.

    Science.gov (United States)

    Ren, Hang; Coughlin, Megan A; Major, Terry C; Aiello, Salvatore; Rojas Pena, Alvaro; Bartlett, Robert H; Meyerhoff, Mark E

    2015-08-18

    A novel electrochemically controlled release method for nitric oxide (NO) (based on electrochemical reduction of nitrite ions) is combined with an amperometric oxygen sensor within a dual lumen catheter configuration for the continuous in vivo sensing of the partial pressure of oxygen (PO2) in blood. The on-demand electrochemical NO generation/release method is shown to be fully compatible with amperometric PO2 sensing. The performance of the sensors is evaluated in rabbit veins and pig arteries for 7 and 21 h, respectively. Overall, the NO releasing sensors measure both venous and arterial PO2 values more accurately with an average deviation of -2 ± 11% and good correlation (R(2) = 0.97) with in vitro blood measurements, whereas the corresponding control sensors without NO release show an average deviation of -31 ± 28% and poor correlation (R(2) = 0.43) at time points >4 h after implantation in veins and >6 h in arteries. The NO releasing sensors induce less thrombus formation on the catheter surface in both veins and arteries (p < 0.05). This electrochemical NO generation/release method could offer a new and attractive means to improve the biocompatibility and performance of implantable chemical sensors.

  1. Covalent modification of multiwalled carbon nanotubes with neutral red for the fabrication of an amperometric hydrogen peroxide sensor

    International Nuclear Information System (INIS)

    Jeykumari, D R Shobha; Narayanan, S Sriman

    2007-01-01

    The nanoscale dimensions, graphitic surface chemistry and electronic properties of multiwalled carbon nanotubes (MWNTs) make them an ideal candidate for chemical and biochemical sensing. In this paper we explore a covalent chemical strategy for functionalization of MWNTs with neutral red through carbodiimide coupling between the primary amine of neutral red and carboxyl groups of the carbon nanotubes. The construction of an amperometric sensor was achieved by abrasive immobilization of the functionalized MWNTs on a paraffin impregnated graphite electrode followed by a coating of a thin film of nafion. The neutral red functionalized MWNTs were characterized by spectroscopic and electroanalytical methods. From the voltammetric studies, MWNTs were found to exhibit a higher accessible surface area in electrochemical reactions. The modified electrode exhibited stable electrocatalytic activity toward hydrogen peroxide reduction in a wide potential range. A significant decrease in overvoltage for the reduction of hydrogen peroxide, as well as a dramatic increase in the peak currents in comparison with a bare graphite electrode were observed. Such an ability of neutral red functionalized carbon nanotubes to promote the hydrogen peroxide electron transfer reaction with a short response time (<4 s) and long-term stability, a low detection limit, an extended linear concentration range and a high sensitivity suggest great promise for dehydrogenase and oxidase based amperometric biosensors

  2. Covalent modification of multiwalled carbon nanotubes with neutral red for the fabrication of an amperometric hydrogen peroxide sensor

    Energy Technology Data Exchange (ETDEWEB)

    Jeykumari, D R Shobha; Narayanan, S Sriman [Department of Analytical Chemistry, School of Chemical Sciences, University of Madras, Guindy Campus, Chennai-600 025 (India)

    2007-03-28

    The nanoscale dimensions, graphitic surface chemistry and electronic properties of multiwalled carbon nanotubes (MWNTs) make them an ideal candidate for chemical and biochemical sensing. In this paper we explore a covalent chemical strategy for functionalization of MWNTs with neutral red through carbodiimide coupling between the primary amine of neutral red and carboxyl groups of the carbon nanotubes. The construction of an amperometric sensor was achieved by abrasive immobilization of the functionalized MWNTs on a paraffin impregnated graphite electrode followed by a coating of a thin film of nafion. The neutral red functionalized MWNTs were characterized by spectroscopic and electroanalytical methods. From the voltammetric studies, MWNTs were found to exhibit a higher accessible surface area in electrochemical reactions. The modified electrode exhibited stable electrocatalytic activity toward hydrogen peroxide reduction in a wide potential range. A significant decrease in overvoltage for the reduction of hydrogen peroxide, as well as a dramatic increase in the peak currents in comparison with a bare graphite electrode were observed. Such an ability of neutral red functionalized carbon nanotubes to promote the hydrogen peroxide electron transfer reaction with a short response time (<4 s) and long-term stability, a low detection limit, an extended linear concentration range and a high sensitivity suggest great promise for dehydrogenase and oxidase based amperometric biosensors.

  3. An Amperometric Biosensor Based on Alanine Dehydrogenase for the Determination of Low Level of Ammonium Ion in Water

    Directory of Open Access Journals (Sweden)

    Tan Ling Ling

    2011-01-01

    Full Text Available An amperometric electrochemical biosensor has been developed for ammonium (NH4+ ion detection by immobilising alanine dehydrogenase (AlaDH enzyme in a photocurable methacrylic membrane made up of poly(2-hydroxyethyl methacrylate (pHEMA on a screen-printed carbon paste electrode (SPE. The current detected was based on the electrocatalytic oxidation of nicotinamide adenine dinucleotide reduced (NADH that is proportional to the consumption of NH4+ ion whilst enzymatic amination of AlaDH and pyruvate is taking place. The biosensor was operated amperometrically at a potential of +0.6 V and optimum pH 7. The NH4+ biosensor demonstrated linear response to NH4+ ion concentration in the range of 0.03–1.02 mg/L with a limit of detection (LOD of 8.52 μg/L. The proposed method has been successfully applied to the determination of NH4+ ion in river water samples without any pretreatment. The levels of possible interferents in the waters were negligible to cause any interference on the proposed method. The analytical performance of the biosensor was comparable to the colorimetric method using Nesslerisation but with much lower detection limit and linear response range at ppb level.

  4. Highly sensitive amperometric biosensor based on electrochemically-reduced graphene oxide-chitosan/hemoglobin nanocomposite for nitromethane determination.

    Science.gov (United States)

    Wen, Yunping; Wen, Wei; Zhang, Xiuhua; Wang, Shengfu

    2016-05-15

    Nitromethane (CH3NO2) is an important organic chemical raw material with a wide variety of applications as well as one of the most common pollutants. Therefore it is pretty important to establish a simple and sensitive detection method for CH3NO2. In our study, a novel amperometric biosensor for nitromethane (CH3NO2) based on immobilization of electrochemically-reduced graphene oxide (rGO), chitosan (CS) and hemoglobin (Hb) on a glassy carbon electrode (GCE) was constructed. Scanning electron microscopy, infrared spectroscopy and electrochemical methods were used to characterize the Hb-CS/rGO-CS composite film. The effects of scan rate and pH of phosphate buffer on the biosensor have been studied in detail and optimized. Due to the graphene and chitosan nanocomposite, the developed biosensor demonstrating direct electrochemistry with faster electron-transfer rate (6.48s(-1)) and excellent catalytic activity towards CH3NO2. Under optimal conditions, the proposed biosensor exhibited fast amperometric response (<5s) to CH3NO2 with a wide linear range of 5 μM~1.46 mM (R=0.999) and a low detection limit of 1.5 μM (S/N=3). In addition, the biosensor had high selectivity, reproducibility and stability, providing the possibility for monitoring CH3NO2 in complex real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Amperometric Gas Sensors as a Low Cost Emerging Technology Platform for Air Quality Monitoring Applications: A Review.

    Science.gov (United States)

    Baron, Ronan; Saffell, John

    2017-11-22

    This review examines the use of amperometric electrochemical gas sensors for monitoring inorganic gases that affect urban air quality. First, we consider amperometric gas sensor technology including its development toward specifically designed air quality sensors. We then review recent academic and research organizations' studies where this technology has been trialed for air quality monitoring applications: early studies showed the potential of electrochemical gas sensors when colocated with reference Air Quality Monitoring (AQM) stations. Spatially dense networks with fast temporal resolution provide information not available from sparse AQMs with longer recording intervals. We review how this technology is being offered as commercial urban air quality networks and consider the remaining challenges. Sensors must be sensitive, selective, and stable; air quality monitors/nodes must be electronically and mechanically well designed. Data correction is required and models with differing levels of sophistication are being designed. Data analysis and validation is possibly the biggest remaining hurdle needed to deliver reliable concentration readings. Finally, this review also considers the roles of companies, urban infrastructure requirements, and public research in the development of this technology.

  6. Amperometric Immunosensor for Carbofuran Detection Based on MWCNTs/GS-PEI-Au and AuNPs-Antibody Conjugate

    Directory of Open Access Journals (Sweden)

    Xiangyou Wang

    2013-04-01

    Full Text Available In this paper, an amperometric immunosensor for the detection of carbofuran was developed. Firstly, multiwall carbon nanotubes (MWCNTs and graphene sheets-ethyleneimine polymer-Au (GS-PEI-Au nanocomposites were modified onto the surface of a glass carbon electrode (GCE via self-assembly. The nanocomposites can increase the surface area of the GCE to capture a large amount of antibody, as well as produce a synergistic effect in the electrochemical performance. Then the modified electrode was coated with gold nanoparticles-antibody conjugate (AuNPs-Ab and blocked with BSA. The monoclonal antibody against carbofuran was covalently immobilized on the AuNPs with glutathione as a spacer arm. The morphologies of the GS-PEI-Au nanocomposites and the fabrication process of the immunosensor were characterized by X-ray diffraction (XRD, ultraviolet and visible absorption spectroscopy (UV-vis and scanning electron microscopy (SEM, respectively. Under optimal conditions, the immunosensor showed a wide linear range, from 0.5 to 500 ng/mL, with a detection limit of 0.03 ng/mL (S/N = 3. The as-constructed immunosensor exhibited notable performance features such as high specificity, good reproducibility, acceptable stability and regeneration performance. The results are mainly due to the excellent properties of MWCNTs, GS-PEI-Au nanocomposites and the covalent immobilization of Ab with free hapten binding sites for further immunoreaction. It provides a new avenue for amperometric immunosensor fabrication.

  7. An enzymatic method for the rapid measurement of the hemoglobin A1c by a flow-injection system comprised of an electrochemical detector with a specific enzyme-reactor and a spectrophotometer

    International Nuclear Information System (INIS)

    Nanjo, Yoko; Hayashi, Ryuzo; Yao, Toshio

    2007-01-01

    A flow-injection analytical (FIA) system, comprised of an electrochemical detector with a fructosyl-peptide oxidase (FPOX-CET) reactor and a flow-type spectrophotometer, was proposed for the simultaneous measurement of glycohemoglobin and total hemoglobin in blood cell. The blood cell samples were hemolyzed with a surfactant and then treated with protease. In the first stage of operation, total hemoglobin in digested sample was determined spectrophotometrically. In the second stage, fructosyl valyl histidine (FVH) released from glycohemoglobin by the selective proteolysis was determined specifically using the electrochemical detector with the FPOX-CET reactor. The FIA system could be automatically processed at an analytical speed of 40 samples per hour. The proposed assay method could determine selectively only the glycated N-terminal residue of β-chain in glycohemoglobin and total hemoglobin in blood cell. The enzymatic hemoglobin A 1c (HbA 1c ) value calculated by the concentration ratio of the FVH to total hemoglobin, was closely correlated with the HbA 1c values certified by the Japan Diabetic Society (JDS) and the International Federation of Clinical Chemistry (IFCC)

  8. Determinação potenciométrica em fluxo de cloreto de cetilpiridinio em desinfectantes bucais Potentiometric determination of cetylpyridinium chloride in oral desinfectants by flow injection analysis

    Directory of Open Access Journals (Sweden)

    Paula C. S. Baptista

    2003-08-01

    Full Text Available The work describes a new procedure for cetylpyridinium chloride determination in oral disinfectants, based on a flow-injection system with potentiometric detection. The determination was based on the measurement of picrate concentration decrease as result of ion-pair reaction with the analyte present in the injected sample. In the optimised set-up the sample injection volume was kept at 400 µL and merged downstream with the reagent solution containing 1,0 x10-5 mol/L of picrate adjusted to pH 5.0 with citrate/citric acid buffer. The flow rate was fixed at 8 mL/min and the reactor length at 40 cm. The proposed procedure enables the determination of cetylpyridinium in the analytical range of 5,0x10-6 - 7,5x10-5 mol/L at a sampling rate of 60/h. The results for real samples had a precision better than 3% and were comparable to the labelled values.

  9. Sensitive determination of perphenazine in pharmaceuticals and human serum by flow injection chemiluminescence method using [Ru(phen){sub 3}]{sup 2+}-Ce(IV) system and a chemometrical optimization approach

    Energy Technology Data Exchange (ETDEWEB)

    Rezaei, B.; Mokhtari, A., E-mail: rezaei@cc.iut.ac.i [Isfahan University of Technology (Iran, Islamic Republic of). Dept. of Chemistry

    2011-07-01

    This paper describes a simple, rapid and sensitive chemiluminescence (CL) method for the determination of perphenazine by flow injection system. All variables that can affect the CL response were optimized by employing central composite design (CCD) for the experimental design and response surface methodology for the modeling. Optimization by means of CCD method with respect to conventional single factor at a time method showed a significant improvement in the sensitivity. Under the optimum experimental conditions, a wide linear relationship between analyte concentration and peak height was obtained within the range 1.2-1,300 ng mL{sup -1} with correlation coefficient of 0.9978. The limit of detection was 0.4 ng mL{sup -1} (S/N = 3) and the relative standard deviation for 6 repeated measurements of a solution containing 70.5 ng mL{sup -1} was lower than 4%. This method was successfully applied for the quantification of perphenazine in pharmaceutical formulations and human serum with good recoveries (95.3-104.0%). Sample throughput was 100 +- 5 samples per hour. (author)

  10. Sensitive determination of perphenazine in pharmaceuticals and human serum by flow injection chemiluminescence method using [Ru(phen)3]2+-Ce(IV) system and a chemometrical optimization approach

    International Nuclear Information System (INIS)

    Rezaei, B.; Mokhtari, A.

    2011-01-01

    This paper describes a simple, rapid and sensitive chemiluminescence (CL) method for the determination of perphenazine by flow injection system. All variables that can affect the CL response were optimized by employing central composite design (CCD) for the experimental design and response surface methodology for the modeling. Optimization by means of CCD method with respect to conventional single factor at a time method showed a significant improvement in the sensitivity. Under the optimum experimental conditions, a wide linear relationship between analyte concentration and peak height was obtained within the range 1.2-1,300 ng mL -1 with correlation coefficient of 0.9978. The limit of detection was 0.4 ng mL -1 (S/N = 3) and the relative standard deviation for 6 repeated measurements of a solution containing 70.5 ng mL -1 was lower than 4%. This method was successfully applied for the quantification of perphenazine in pharmaceutical formulations and human serum with good recoveries (95.3-104.0%). Sample throughput was 100 +- 5 samples per hour. (author)

  11. Calibration and fluctuation of the secular frequency peak amplitude versus initial condition distribution of the ion cloud confined into a three-dimensional quadrupole ion trap using a fourier transform operating mode and a steady ion flow injection mode

    International Nuclear Information System (INIS)

    Janulyte, A.; Andre, J.; Carette, M.; Mercury, M.; Reynard, C; Zerega, Y.

    2009-01-01

    A specific Fourier transform operating mode is applied to a 3-dimensional quadrupolar ion trap for mass analysis (Fourier Transform Quadrupolar Ion Trap (FTQIT) Operating Mode or Mass Spectrometer). With this operating mode, an image signal, which is representative of the collective motion of simultaneously confined ions, is made up from a set of recorded time-of-flight histograms. In an ion trap, the secular frequency of ion motion depends on m/Z ratio of the ion. By Fourier transformation of the image signal, one observes the frequency peak of each confined ionic species. When only one ionic species is confined, the peak amplitude is proportional to the maximal amplitude of the image signal. The maximal amplitude of the image signal is expressed according to the operating parameters, the initial conditions of the ions and the number of ions. Simulation tools lead to fluctuation calculation of the maximal amplitude of the image signal. Two origins are explored: (1) the fluctuation of the numbers of ions according to the steady ion flow injection mode (SIFIM) used with this operating mode and (2) the distribution fluctuation of the initial positions and velocities. Initial confinement conditions, obtained with SIFIM injection mode, lead to optimal detection with small fluctuations of the peak amplitude for Fourier transform operating mode applied to an ion trap. (authors)

  12. Amperometric cell for subcutaneous detection of hydrogen sulfide in anesthetized experimental animals

    International Nuclear Information System (INIS)

    Nagy, L; Nagy, G; Filotás, D; Boros, M; Pozsgai, G; Pintér, E

    2014-01-01

    Hydrogen sulfide (H 2 S) is a toxic gas. It has been recognized that H 2 S evolving in biochemical reactions in living organisms has an important role in different physiologic processes. Nowadays, H 2 S is known as an endogenous messenger molecule. Natural sulfurous spring water has been proved beneficial in the therapy of diseases of the skin and other organs (Boros et al 2013). In vivo real-time detection of local H 2 S concentration is an important but challenging task. We developed a two-electrode amperometric cell for selective subcutaneous detection of H 2 S in anesthetized mice. The cell is a small size implantable gas sensor containing a platinum disc anode and a silver cathode. The selectivity is provided by a membrane permeable only by gases. There is a buffered reversible electrochemical mediator solution in an oxidized form inside the cell. As gaseous H 2 S penetrates into the cell the mediator is reduced, and +0.4 V versus the reference is employed on the platinum working electrode. The reduced mediator is oxidized on the anode surface. The current provides an analytical signal representing the concentration of H 2 S. Appropriate shape, size and membrane material were selected, and optimal working parameters—such as mediator concentration, pH and cell voltage—were determined in vitro. The lower limit of detection in the stirred sample solution at pH = 5.5 was as small as 9.4  ×  10 −7  M and a dynamic concentration range of 0–6  ×  10 –4  M could be achieved. The detecting surfaces of the cell were covered with freshly dissected mouse skin to test dermal H 2 S permeability. In other experiments, the cell was implanted subcutaneously in an anesthetized mouse and the animal was submerged in a buffer solution containing different concentrations of H 2 S so that the skin surface over the sensor was covered by the solution. Measurements of subcutaneous H 2 S concentration were taken. The experiments clearly proved that H 2 S

  13. Flow Injection Spectrophotometric Determination of Glyphosate ...

    African Journals Online (AJOL)

    NICOLAAS

    limits and causes digestive tract irritation, eyes and skin irrita- tion, low blood ... techniques, mostly chromatographic, have been developed for ... enhanced photochemically induced fluorescence (MEPIF) .... with glyphosate on the same field or in the nearby fields. .... At 700 µL sample volume two peaks near to each.

  14. Development of an on-line flow injection Sr/matrix separation method for accurate, high-throughput determination of Sr isotope ratios by multiple collector-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Galler, Patrick; Limbeck, Andreas; Boulyga, Sergei F; Stingeder, Gerhard; Hirata, Takafumi; Prohaska, Thomas

    2007-07-01

    This work introduces a newly developed on-line flow injection (FI) Sr/Rb separation method as an alternative to the common, manual Sr/matrix batch separation procedure, since total analysis time is often limited by sample preparation despite the fast rate of data acquisition possible by inductively coupled plasma-mass spectrometers (ICPMS). Separation columns containing approximately 100 muL of Sr-specific resin were used for on-line FI Sr/matrix separation with subsequent determination of (87)Sr/(86)Sr isotope ratios by multiple collector ICPMS. The occurrence of memory effects exhibited by the Sr-specific resin, a major restriction to the repetitive use of this costly material, could successfully be overcome. The method was fully validated by means of certified reference materials. A set of two biological and six geological Sr- and Rb-bearing samples was successfully characterized for its (87)Sr/(86)Sr isotope ratios with precisions of 0.01-0.04% 2 RSD (n = 5-10). Based on our measurements we suggest (87)Sr/(86)Sr isotope ratios of 0.713 15 +/- 0.000 16 (2 SD) and 0.709 31 +/- 0.000 06 (2 SD) for the NIST SRM 1400 bone ash and the NIST SRM 1486 bone meal, respectively. Measured (87)Sr/(86)Sr isotope ratios for five basalt samples are in excellent agreement with published data with deviations from the published value ranging from 0 to 0.03%. A mica sample with a Rb/Sr ratio of approximately 1 was successfully characterized for its (87)Sr/(86)Sr isotope signature to be 0.718 24 +/- 0.000 29 (2 SD) by the proposed method. Synthetic samples with Rb/Sr ratios of up to 10/1 could successfully be measured without significant interferences on mass 87, which would otherwise bias the accuracy and uncertainty of the obtained data.

  15. Determination of inorganic mercury and total mercury in biological and environmental samples by flow injection-cold vapor-atomic absorption spectrometry using sodium borohydride as the sole reducing agent

    International Nuclear Information System (INIS)

    Rio Segade, Susana; Tyson, Julian F.

    2003-01-01

    A simple, fast, precise and accurate method to determine inorganic mercury and total mercury in biological and environmental samples was developed. The optimized flow-injection mercury system permitted the separate determination of inorganic mercury and total mercury using sodium borohydride as reducing agent. Inorganic mercury was selectively determined after reduction with 10 -4 % w/v sodium borohydride, while total mercury was determined after reduction with 0.75% w/v sodium borohydride. The calibration graphs were linear up to 30 ng ml -1 . The detection limits of the method based on three times the standard deviation of the blank were 24 and 3.9 ng l -1 for total mercury and inorganic mercury determination, respectively. The relative standard deviation was less than 1.5% for a 10 ng ml -1 mercury standard. As a means of checking method performance, deionized water and pond water samples were spiked with methylmercury and inorganic mercury; quantitative recovery for total mercury and inorganic mercury was obtained. The accuracy of the method was verified by analyzing alkaline and acid extracts of five biological and sediment reference materials. Microwave-assisted extraction procedures resulted in higher concentrations of recovered mercury species, lower matrix interference with mercury determination and less time involved in sample treatment than conventional extraction procedures. The standard addition method was only needed for calibration when biological samples were analyzed. The detection limits were in the range of 1.2-19 and 6.6-18 ng g -1 in biological and sediment samples for inorganic mercury and total mercury determination, respectively

  16. Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis.

    Science.gov (United States)

    Quaresma, Maria Cristina Baptista; de Carvalho, Maria de Fátima Batista; Meirelles, Francis Assis; Santiago, Vânia Maria Junqueira; Santelli, Ricardo Erthal

    2007-02-01

    A sample preparation procedure for the quantitative determination of free and total cyanides in industrial effluents has been developed that involves hydrocyanic acid vapor generation via focused microwave radiation. Hydrocyanic acid vapor was generated from free cyanides using only 5 min of irradiation time (90 W power) and a purge time of 5 min. The HCN generated was absorbed into an accepting NaOH solution using very simple glassware apparatus that was appropriate for the microwave oven cavity. After that, the cyanide concentration was determined within 90 s using a well-known spectrophotometric flow injection analysis system. Total cyanide analysis required 15 min irradiation time (90 W power), as well as chemical conditions such as the presence of EDTA-acetate buffer solution or ascorbic acid, depending on the effluent to be analyzed (petroleum refinery or electroplating effluents, respectively). The detection limit was 0.018 mg CN l(-1) (quantification limit of 0.05 mg CN l(-1)), and the measured RSD was better than 8% for ten independent analyses of effluent samples (1.4 mg l(-1) cyanide). The accuracy of the procedure was assessed via analyte spiking (with free and complex cyanides) and by performing an independent sample analysis based on the standard methodology recommended by the APHA for comparison. The sample preparation procedure takes only 10 min for free and 20 min for total cyanide, making this procedure much faster than traditional methodologies (conventional heating and distillation), which are time-consuming (they require at least 1 h). Samples from oil (sour and stripping tower bottom waters) and electroplating effluents were analyzed successfully.

  17. Amperometric biosensor based on carbon nanotubes coated with polyaniline/dendrimer-encapsulated Pt nanoparticles for glucose detection

    International Nuclear Information System (INIS)

    Xu Lihuan; Zhu Yihua; Yang Xiaoling; Li Chunzhong

    2009-01-01

    A novel amperometric glucose biosensor based on the nanocomposites of multi-wall carbon nanotubes (CNT) coated with polyaniline (PANI) and dendrimer-encapsulated Pt nanoparticles (Pt-DENs) is prepared. CNT coated with protonated PANI is in situ synthesized and Pt-DENs is absorbed on PANI/CNT composite surface by self-assembly method. Then Glucose oxidase (GOx) is crosslink-immobilizated onto Pt-DENs/PANI/CNT composite film. The results show that the fabricated GOx/Pt-DENs/PANI/CNT electrode exhibits excellent response performance to glucose, such as low detection limit (0.5 μM), wide linear range (1 μM-12 mM), short response time (about 5 s), high sensitivity (42.0 μA mM -1 cm -2 ) and stability (83% remains after 3 weeks).

  18. Determination of Patulin Using Amperometric Tyrosinase Biosensors Based on Electrodes Modified with Carbon Nanotubes and Gold Nanoparticles

    Directory of Open Access Journals (Sweden)

    R.M. Varlamova

    2016-06-01

    Full Text Available New amperometric biosensors based on platinum screen printed electrodes modified with multi-walled carbon nanotubes, gold nanoparticles, and immobilized enzyme – tyrosinase have been developed for determination of patulin in the concentrations of 1·10–6 – 8·10–12 mol/L with an error of no more than 0.063. The best conditions for obtaining gold nanoparticles have been chosen. The conditions for immobilization of multi-walled carbon nanotubes and gold nanoparticles on the surface of the planar electrode have been revealed. The conditions for functioning of the proposed biosensors have been identified. The results have been used to control the content of patulin in food products within and lower than the maximum allowable levels.

  19. Amperometric Detection of Sub-ppm Formaldehyde Using Single-Walled Carbon Nanotubes and Hydroxylamines: A Referenced Chemiresistive System.

    Science.gov (United States)

    Ishihara, Shinsuke; Labuta, Jan; Nakanishi, Takashi; Tanaka, Takeshi; Kataura, Hiromichi

    2017-10-27

    We report amperometric detection of formaldehyde (HCHO) using hydroxylamine hydrochloride and single-walled carbon nanotubes (SWCNTs). Hydroxylamine hydrochloride reacts with HCHO to emit HCl vapor, which injects a hole carrier into semiconducting SWCNTs. The increase of conductivity in SWCNTs is easily monitored using an ohmmeter. The debundling of SWCNTs with a metallo-supramolecular polymer (MSP) increased the active surface area in the SWCNTs network, leading to excellent sensitivity to HCHO with a limit of detection (LoD) of 0.016 ppm. The response of sensor is reversible, and the sensor is reusable. The selectivity to HCHO is 10 5 -10 6 times higher than interferences with other volatiles such as water, methanol, and toluene. Moreover, false-positive responses caused by a significant variation of humidity and/or temperature are successfully discriminated from true-positive responses by using two sensors, one with and the other without hydroxylamine hydrochloride, in a referenced system.

  20. Fuel cell-powered microfluidic platform for lab-on-a-chip applications: Integration into an autonomous amperometric sensing device.

    Science.gov (United States)

    Esquivel, J P; Colomer-Farrarons, J; Castellarnau, M; Salleras, M; del Campo, F J; Samitier, J; Miribel-Català, P; Sabaté, N

    2012-11-07

    The present paper reports for the first time the integration of a microfluidic system, electronics modules, amperometric sensor and display, all powered by a single micro direct methanol fuel cell. In addition to activating the electronic circuitry, the integrated power source also acts as a tuneable micropump. The electronics fulfil several functions. First, they regulate the micro fuel cell output power, which off-gas controls the flow rate of different solutions toward an electrochemical sensor through microfluidic channels. Secondly, as the fuel cell powers a three-electrode electrochemical cell, the electronics compare the working electrode output signal with a set reference value. Thirdly, if the concentration measured by the sensor exceeds this threshold value, the electronics switch on an integrated organic display. This integrated approach pushes forward the development of truly autonomous point-of-care devices relying on electrochemical detection.

  1. Amperometric sensor for detection of bisphenol A using a pencil graphite electrode modified with polyaniline nanorods and multiwalled carbon nanotubes

    International Nuclear Information System (INIS)

    Poorahong, S.; Thammakhet, C.; Numnuam, A.; Kanatharana, P.; Thavarungkul, P.; Limbut, W.

    2012-01-01

    We report on a simple and highly sensitive amperometric method for the determination of bisphenol A (BPA) using pencil graphite electrodes modified with polyaniline nanorods and multiwalled carbon nanotubes. The modified electrodes display enhanced electroactivity for the oxidation of BPA compared to the unmodified pencil graphite electrode. Under optimized conditions, the sensor has a linear response to BPA in the 1. 0 and 400 μM concentration range, with a limit of detection of 10 nM (at S/N = 3). The modified electrode also has a remarkably stable response, and up to 95 injections are possible with a relative standard deviation of 4. 2% at 100 μM of BPA. Recoveries range from 86 to 102% for boiling water spiked with BPA from four brands of baby bottles. (author)

  2. Amperometric xanthine biosensors using glassy carbon electrodes modified with electrografted porous silica nanomaterials loaded with xanthine oxidase

    International Nuclear Information System (INIS)

    Saadaoui, Maroua; Sánchez, Alfredo; Díez, Paula; Raouafi, Noureddine; Pingarrón, José M.; Villalonga, Reynaldo

    2016-01-01

    Glassy carbon electrodes were modified with silica materials such as silica nanoparticles, mesoporous silica nanoparticles and mesoporous silica thin films with the aim to introduce scaffolds suitable for the immobilization of enzymes. Xanthine oxidase was selected as a model enzyme, and xanthine as the target analyte. A comparison of the modified electrodes showed the biosensor prepared with mesoporous silica nanoparticles to perform best. By using the respective biosensor, xanthine can be amperometrically determined (via measurement of enzymatically formed hydrogen peroxide) at a working voltage of 0.7 V (vs. Ag/AgCl) with a 0.28 μM detection limit. The biosensor was evaluated in terms of potential interferences, reproducibility and stability, and applied to the determination of fish freshness via sensing of xanthine. (author)

  3. Amperometric glucose biosensor based on glucose oxidase dispersed in multiwalled carbon nanotubes/graphene oxide hybrid biocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Palanisamy, Selvakumar; Cheemalapati, Srikanth; Chen, Shen-Ming, E-mail: smchen78@ms15.hinet.net

    2014-01-01

    An amperometric glucose biosensor based on enhanced and fast direct electron transfer (DET) of glucose oxidase (GOx) at enzyme dispersed multiwalled carbon nanotubes/graphene oxide (MWCNT/GO) hybrid biocomposite was developed. The fabricated hybrid biocomposite was characterized by transmission electron microscopy (TEM), Raman and infrared spectroscopy (IR). The TEM image of hybrid biocomposite reveals that a thin layer of GOx was covered on the surface of MWCNT/GO hybrid composite. IR results validate that the hybrid biocomposite was formed through the electrostatic interactions between GOx and MWCNT/GO hybrid composite. Further, MWCNT/GO hybrid composite has also been characterized by TEM and UV–visible spectroscopy. A pair of well-defined redox peak was observed for GOx immobilized at the hybrid biocomposite electrode than that immobilized at the MWCNT modified electrode. The electron transfer rate constant (K{sub s}) of GOx at the hybrid biocomposite was calculated to be 11.22 s{sup −1}. The higher K{sub s} value revealed that fast DET of GOx occurred at the electrode surface. Moreover, fabricated biosensor showed a good sensitivity towards glucose oxidation over a linear range 0.05–23.2 mM. The limit of detection (LOD) was estimated to be 28 μM. The good features of the proposed biosensor could be used for the accurate detection of glucose in the biological samples. - Highlights: • An amperometric glucose biosensor has been developed at MWCNT/GO hybrid biocomposite. • Enhanced and fast direct electron transfer kinetics of glucose oxidase has been achieved at hybrid biocomposite. • Hybrid biocomposite has been characterized by TEM, IR and Raman spectroscopy. • Highly sensitive and selective for glucose determination.

  4. In vivo continuous and simultaneous monitoring of brain energy substrates with a multiplex amperometric enzyme-based biosensor device.

    Science.gov (United States)

    Cordeiro, C A; de Vries, M G; Ngabi, W; Oomen, P E; Cremers, T I F H; Westerink, B H C

    2015-05-15

    Enzyme-based amperometric biosensors are widely used for monitoring key biomarkers. In experimental neuroscience there is a growing interest in in vivo continuous and simultaneous monitoring of metabolism-related biomarkers, like glucose, lactate and pyruvate. The use of multiplex biosensors will provide better understanding of brain energy metabolism and its role in neuropathologies such as diabetes, ischemia, and epilepsy. We have developed and characterized an implantable multiplex microbiosensor device (MBD) for simultaneous and continuous in vivo monitoring of glucose, lactate, and pyruvate. First, we developed and characterized amperometric microbiosensors for monitoring lactate and pyruvate. In vitro evaluation allowed us to choose the most suitable biosensors for incorporation into the MBD, along with glucose and background biosensors. Fully assembled MBDs were characterized in vitro. The calculated performance parameters (LOD, LR, LRS, IMAX and appKM) showed that the multiplex MBD was highly selective and sensitive (LRS≥100 nA/mM) for each analyte and within an adequate range for in vivo application. Finally, MBDs were implanted in the mPFC of anesthetized adult male Wistar rats for in vivo evaluation. Following an equilibration period, baseline brain levels of glucose (1.3±0.2 mM), lactate (1.5±0.4 mM) and pyruvate (0.3±0.1 mM) were established. Subsequently, the MBDs recorded the responses of the animals when submitted to hyperglycemic (40% glucose i.v.) and hypoglycemic (5 U/kg insulin i.v.) challenges. Afterwards, MBDs were recalibrated to convert electrochemical readings into accurate substrate concentrations and to assess biofouling. The presented MBD can monitor simultaneously multiple biomarkers in vivo. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Amperometric glucose biosensor based on glucose oxidase dispersed in multiwalled carbon nanotubes/graphene oxide hybrid biocomposite

    International Nuclear Information System (INIS)

    Palanisamy, Selvakumar; Cheemalapati, Srikanth; Chen, Shen-Ming

    2014-01-01

    An amperometric glucose biosensor based on enhanced and fast direct electron transfer (DET) of glucose oxidase (GOx) at enzyme dispersed multiwalled carbon nanotubes/graphene oxide (MWCNT/GO) hybrid biocomposite was developed. The fabricated hybrid biocomposite was characterized by transmission electron microscopy (TEM), Raman and infrared spectroscopy (IR). The TEM image of hybrid biocomposite reveals that a thin layer of GOx was covered on the surface of MWCNT/GO hybrid composite. IR results validate that the hybrid biocomposite was formed through the electrostatic interactions between GOx and MWCNT/GO hybrid composite. Further, MWCNT/GO hybrid composite has also been characterized by TEM and UV–visible spectroscopy. A pair of well-defined redox peak was observed for GOx immobilized at the hybrid biocomposite electrode than that immobilized at the MWCNT modified electrode. The electron transfer rate constant (K s ) of GOx at the hybrid biocomposite was calculated to be 11.22 s −1 . The higher K s value revealed that fast DET of GOx occurred at the electrode surface. Moreover, fabricated biosensor showed a good sensitivity towards glucose oxidation over a linear range 0.05–23.2 mM. The limit of detection (LOD) was estimated to be 28 μM. The good features of the proposed biosensor could be used for the accurate detection of glucose in the biological samples. - Highlights: • An amperometric glucose biosensor has been developed at MWCNT/GO hybrid biocomposite. • Enhanced and fast direct electron transfer kinetics of glucose oxidase has been achieved at hybrid biocomposite. • Hybrid biocomposite has been characterized by TEM, IR and Raman spectroscopy. • Highly sensitive and selective for glucose determination

  6. A green synthetic strategy of nickel hexacyanoferrate nanoparticals supported on the graphene substrate and its non-enzymatic amperometric sensing application

    Science.gov (United States)

    xue, Zhonghua; He, Nan; Rao, Honghong; Hu, Chenxian; Wang, Xiaofen; Wang, Hui; Liu, Xiuhui; Lu, Xiaoquan

    2017-02-01

    Rapid glucose detection is a key requirement for both diagnosis and treatment of diabetes. A facile and green strategy to achieve spherical-shaped nickel hexacyanoferrate (NiHCF) nanoparticals supported on electrochemical reduction graphene oxide by using electrochemical cyclic voltammetry is explored. As a sensing substrate, electrochemical reduction graphene oxide deposited on a glassy carbon electrode surface exhibited obvious positive effect on the electrodeposition of NiHCF nanoparticals with spherical structure and thus effectively improved the electrical conductivity and electrochemical sensing of the proposed amperometric sensor. Proof-concept experiments demonstrated that the proposed nanocomposites modified electrode exhibited excellent sensitivity toward glucose oxidation as well as with a satisfying detection limit of 0.11 μM. More importantly, we also explore that as a simple, green and facile method, electrochemical technology can be employed and provide a new strategy for developing GO and metal hexacyanoferrate based amperometric sensing platform toward glucose and other biomolecules.

  7. An amperometric penicillin biosensor with enhanced sensitivity based on co-immobilization of carbon nanotubes, hematein, and β-lactamase on glassy carbon electrode

    International Nuclear Information System (INIS)

    Chen Bi; Ma Ming; Su Xiaoli

    2010-01-01

    An amperometric penicillin biosensor with enhanced sensitivity was successfully developed by co-immobilization of multi-walled carbon nanotubes (MWCNTs), hematein, and β-lactamase on glassy carbon electrode using a layer-by-layer assembly technique. Under catalysis of the immobilized enzyme, penicillin was hydrolyzed, decreasing the local pH. The pH change was monitored amperometrically with hematein as a pH-sensitive redox probe. MWCNTs were used as an electron transfer enhancer as well as an efficient immobilization matrix for the sensitivity enhancement. The effects of immobilization procedure, working potential, enzyme quantity, buffer concentration, and sample matrix were investigated. The biosensor offered a minimum detection limit of 50 nM (19 μg L -1 ) for penicillin V, lower than those of the conventional pH change-based biosensors by more than two orders of magnitude. The electrode-to-electrode variation of the response sensitivity was 7.0% RSD.

  8. Comparison between a Direct-Flow SPR Immunosensor for Ampicillin and a Competitive Conventional Amperometric Device: Analytical Features and Possible Applications to Real Samples

    Science.gov (United States)

    Tomassetti, Mauro; Merola, Giovanni; Martini, Elisabetta; Campanella, Luigi; Sanzò, Gabriella; Favero, Gabriele; Mazzei, Franco

    2017-01-01

    In this research, we developed a direct-flow surface plasmon resonance (SPR) immunosensor for ampicillin to perform direct, simple, and fast measurements of this important antibiotic. In order to better evaluate the performance, it was compared with a conventional amperometric immunosensor, working with a competitive format with the aim of finding out experimental real advantages and disadvantages of two respective methods. Results showed that certain analytical features of the new SPR immunodevice, such as the lower limit of detection (LOD) value and the width of the linear range, are poorer than those of a conventional amperometric immunosensor, which adversely affects the application to samples such as natural waters. On the other hand, the SPR immunosensor was more selective to ampicillin, and measurements were more easily and quickly attained compared to those performed with the conventional competitive immunosensor. PMID:28394296

  9. The use of different glucose oxidases for the development of an amperometric reagentless glucose biosensor based on gold nanoparticles covered by polypyrrole

    International Nuclear Information System (INIS)

    German, Natalija; Kausaite-Minkstimiene, Asta; Ramanavicius, Arunas; Semashko, Tatiana; Mikhailova, Raisa; Ramanaviciene, Almira

    2015-01-01

    Graphical abstract: Display Omitted -- ABSTRACT: The amperometric glucose biosensors based on adsorbed electron transfer mediator (ETM) tetrathiafulvalene (TTF) or 1,10-phenanthroline-5,6-dione (PD) and glucose oxidase (GOx) from Aspergillus niger (GOx A.niger ), Penicillium adametzii (GOx P.adametzii ) or Penicillium funiculosum (GOx P.funiculosum ) cross-linked with glutaraldehyde were investigated. ETM and enzyme were immobilized layer by layer on bare graphite rod electrode (GR) premodified with gold nanoparticles (AuNP) of (i) 3.5 nm (GOx/ETM/AuNP 3.5 /GR), (ii) 6.0 nm (GOx/ETM/AuNP 6.0 /GR) and (iii) 13.0 nm (GOx/ETM/AuNP 13.0 /GR) size. The amperometric signals for all the developed biosensors were higher using PD in comparison with TTF. The biosensor based on GOx P.funiculosum showed higher analytical signal to glucose in a comparison to biosensors based on GOx A.niger and GOx P.adametzii . The registered current to glucose using GOx P.funiculosum /PD/AuNP 3.5 /GR electrode was linear in the glucose range from 0.1 to 10.0 mmol L −1 and the limit of detection was 0.024 mmol L −1 . Enzymatical synthesis of polypyrrole (Ppy) layer on the electrode was applied in order to expand the linear glucose detection range. After 22 h of polymerization the amperometric signal was linear in the glucose concentration range from 0.1 to 25.0 mmol L −1 , while after 69 h this rage was increased up to 50.0 mmol L −1 . Additionally Ppy layer on the electrode surface reduced the influence of interfering species on the amperometric signal. The performance of developed biosensor was investigated in human serum samples

  10. Simultaneous determination of 13 carbohydrates using high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry.

    Science.gov (United States)

    Zhao, Dan; Feng, Feng; Yuan, Fei; Su, Jin; Cheng, Yan; Wu, Hanqiu; Song, Kun; Nie, Bo; Yu, Lian; Zhang, Feng

    2017-04-01

    A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2  μg/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Flow injection electrochemical hydride generation inductively coupled plasma time-of-flight mass spectrometry for the simultaneous determination of hydride forming elements and its application to the analysis of fresh water samples

    International Nuclear Information System (INIS)

    Bings, Nicolas H.; Stefanka, Zsolt; Mallada, Sergio Rodriguez

    2003-01-01

    A flow injection (FI) method was developed using electrochemical hydride generation (EcHG) as a sample introduction system, coupled to an inductively coupled plasma time-of-flight mass spectrometer (ICP-TOFMS) for rapid and simultaneous determination of six elements forming hydrides (As, Bi, Ge, Hg, Sb and Se). A novel low volume electrolysis cell, especially suited for FI experiments was designed and the conditions for simultaneous electrochemical hydride generation (EcHG; electrolyte concentrations and flow rates, electrolysis voltage and current) as well as the ICP-TOFMS operational parameters (carrier gas flow rate, modulation pulse width (MPW)) for the simultaneous determination of 12 isotopes were optimized. The compromise operation parameters of the electrolysis were found to be 1.4 and 3 ml min -1 for the anolyte and catholyte flow rates, respectively, using 2 M sulphuric acid. An optimum electrolysis current of 0.7 A (16 V) and an argon carrier gas flow rate of 0.91 l min -1 were chosen. A modulation pulse width of 5 μs, which influences the sensitivity through the amount of ions being collected by the MS per single analytical cycle, provided optimum results for the detection of transient signals. The achieved detection limits were compared with those obtained by using FI in combination with conventional nebulization (FI-ICP-TOFMS); values for chemical hydride generation (FI-CHG-ICP-TOFMS) were taken from the literature. By using a 200 μl sample loop absolute detection limits (3σ) in the range of 10-160 pg for As, Bi, Ge, Hg, Sb and 1.1 ng for Se and a precision of 4-8% for seven replicate injections of 20-100 ng ml -1 multielemental sample solutions were achieved. The analysis of a standard reference material (SRM) 1643d (NIST, 'Trace Elements in Water') showed good agreement with the certified values for As and Sb. Se showed a drastic difference, which is probably due to the presence of hydride-inactive Se species in the sample. Recoveries better than

  12. Magnetic Beads-Based Sensor with Tailored Sensitivity for Rapid and Single-Step Amperometric Determination of miRNAs

    Directory of Open Access Journals (Sweden)

    Eva Vargas

    2017-11-01

    Full Text Available This work describes a sensitive amperometric magneto-biosensor for single-step and rapid determination of microRNAs (miRNAs. The developed strategy involves the use of direct hybridization of the target miRNA (miRNA-21 with a specific biotinylated DNA probe immobilized on streptavidin-modified magnetic beads (MBs, and labeling of the resulting heteroduplexes with a specific DNA–RNA antibody and the bacterial protein A (ProtA conjugated with an horseradish peroxidase (HRP homopolymer (Poly-HRP40 as an enzymatic label for signal amplification. Amperometric detection is performed upon magnetic capture of the modified MBs onto the working electrode surface of disposable screen-printed carbon electrodes (SPCEs using the H2O2/hydroquinone (HQ system. The magnitude of the cathodic signal obtained at −0.20 V (vs. the Ag pseudo-reference electrode demonstrated linear dependence with the concentration of the synthetic target miRNA over the 1.0 to 100 pM range. The method provided a detection limit (LOD of 10 attomoles (in a 25 μL sample without any target miRNA amplification in just 30 min (once the DNA capture probe-MBs were prepared. This approach shows improved sensitivity compared with that of biosensors constructed with the same anti-DNA–RNA Ab as capture instead of a detector antibody and further labeling with a Strep-HRP conjugate instead of the Poly-HRP40 homopolymer. The developed strategy involves a single step working protocol, as well as the possibility to tailor the sensitivity by enlarging the length of the DNA/miRNA heteroduplexes using additional probes and/or performing the labelling with ProtA conjugated with homopolymers prepared with different numbers of HRP molecules. The practical usefulness was demonstrated by determination of the endogenous levels of the mature target miRNA in 250 ng raw total RNA (RNAt extracted from human mammary epithelial normal (MCF-10A and cancer (MCF-7 cells and tumor tissues.

  13. Radiometric detection in flow-injection analysis; Radiometric flow-injection analysis

    Energy Technology Data Exchange (ETDEWEB)

    Myint, U; Han, B; Myoe, K M; Kywe, A; Thida, [Yangon Univ. (Myanmar). Dept. of Chemistry; Toelgyessy, J [Slovak Technical Univ., Braatislava (Slovakia). Dept. of Environmental Science

    1994-05-17

    A single line system with a detector of radioactivity was used for the determination of [sup 60]Co. In the determination, no additional chemistry is involved and limited dispersion is desirable. For this application, the FIA system is used only as a transport system for the sample up to the detector. (author) 7 refs.; 4 figs.

  14. On the Electrooxidation and Amperometric Detection of NO Gas at the Pt/Nafion® Electrode

    Directory of Open Access Journals (Sweden)

    Jin-Cherng Yang

    2003-08-01

    Full Text Available The electrochemical oxidation of nitric oxide (NO gas at the Pt/Nafion® electrode has been studied at a concentration of 500 ppm. The electrooxidation of NO taking place over a wide potential range can be described by a transcendental equation, from which the half-wave potential of the reaction can be determined. For NO oxidation with appreciable overpotentials but negligible mass-transfer effects, the Tafel kinetics applies. The obtained charge transfer coefficient (a and the exchange current density (io are 0.77 and 14 mA/cm2, respectively. An amperometric NO gas sensor based on the Pt/Nafion® electrode has been fabricated and tested over the NO concentration range from 0 to 500 ppm. The Pt/Nafion® electrode was used as an anode at a fixed potential, preferably 1.15 V (vs. Ag/AgCl/sat. KCl, which assures current limitation by diffusion only. The sensitivity of the electrochemical sensor was found to be 1.86 mA/ppm/cm2. The potential interference by other gases, such as nitrogen dioxide (NO2 and carbon monoxide (CO, was also studied in the range 0-500 ppm. Both sensitivity for NO and selectivity of NO over NO2/CO show significant enhancement upon using a cyclic voltammetric (CV activation, or cleaning procedure.

  15. Amperometric glucose biosensor based on layer-by-layer films of microperoxidase-11 and liposome-encapsulated glucose oxidase.

    Science.gov (United States)

    Graça, J S; de Oliveira, R F; de Moraes, M L; Ferreira, M

    2014-04-01

    An important step in several bioanalytical applications is the immobilization of biomolecules. Accordingly, this procedure must be carefully chosen to preserve their biological structure and fully explore their properties. For this purpose, we combined the versatility of the layer-by-layer (LbL) method for the immobilization of biomolecules with the protective behavior of liposome-encapsulated systems to fabricate a novel amperometric glucose biosensor. To obtain the biosensing unit, an LbL film of the H2O2 catalyst polypeptide microperoxidase-11 (MP-11) was assembled onto an indium-tin oxide (ITO) electrode followed by the deposition of a liposome-encapsulated glucose oxidase (GOx) layer. The biosensor response toward glucose detection showed a sensitivity of 0.91±0.09 (μA/cm2)/mM and a limit of detection (LOD) of 8.6±1.1 μM, demonstrating an improved performance compared to similar biosensors with a single phospholipid-liposome or even containing a non-encapsulated GOx layer. Finally, glucose detection was also performed in a zero-lactose milk sample to demonstrate the potential of the biosensor for food analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Mediatorless amperometric bienzyme glucose biosensor based on horseradish peroxidase and glucose oxidase cross-linked to multiwall carbon nanotubes

    International Nuclear Information System (INIS)

    Xu, Shuxia; Zhou, Shiyi; Zhang, Xinfeng; Qi, Honglan; Zhang, Chengxiao

    2014-01-01

    We report on a bienzyme-channeling sensor for sensing glucose without the aid of mediator. It was fabricated by cross-linking horseradish peroxidase (HRP) and glucose oxidase (GOx) on a glassy carbon electrode modified with multiwalled carbon nanotubes (MWNTs). The bienzyme was cross-linked with the MWNTs by glutaraldehyde and bovine serum albumin. The MWNTs were employed to accelerate the electron transfer between immobilized HRP and electrode. Glucose was sensed by amperometric reduction of enzymatically generated H 2 O 2 at an applied voltage of −50 mV (vs. Ag/AgCl). Factors influencing the preparation and performance of the bienzyme electrode were investigated in detail. The biosensor exhibited a fast and linear response to glucose in the concentration range from 0.4 to 15 mM, with a detection limit of 0.4 mM. The sensor exhibited good selectivity and durability, with a long-term relative standard deviation of <5 %. Analysis of glucose-spiked human serum samples yielded recoveries between 96 and 101 %. (author)

  17. Influence of aspect ratio and surface defect density on hydrothermally grown ZnO nanorods towards amperometric glucose biosensing applications

    Science.gov (United States)

    Shukla, Mayoorika; Pramila; Dixit, Tejendra; Prakash, Rajiv; Palani, I. A.; Singh, Vipul

    2017-11-01

    In this work, hydrothermally grown ZnO Nanorods Array (ZNA) has been synthesized over Platinum (Pt) coated glass substrate, for biosensing applications. In-situ addition of strong oxidizing agent viz KMnO4 during hydrothermal growth was found to have profound effect on the physical properties of ZNA. Glucose oxidase (GOx) was later immobilized over ZNA by means of physical adsorption process. Further influence of varying aspect ratio, enzyme loading and surface defects on amperometric glucose biosensor has been analyzed. Significant variation in biosensor performance was observed by varying the amount of KMnO4 addition during the growth. Moreover, investigations revealed that the suppression of surface defects and aspect ratio variation of the ZNA played key role towards the observed improvement in the biosensor performance, thereby significantly affecting the sensitivity and response time of the fabricated biosensor. Among different biosensors fabricated having varied aspect ratio and surface defect density of ZNA, the best electrode resulted into sensitivity and response time to be 18.7 mA cm-2 M-1 and <5 s respectively. The observed results revealed that apart from high aspect ratio nanostructures and the extent of enzyme loading, surface defect density also hold a key towards ZnO nanostructures based bio-sensing applications.

  18. Amperometric glucose biosensor based on glucose oxidase dispersed in multiwalled carbon nanotubes/graphene oxide hybrid biocomposite.

    Science.gov (United States)

    Palanisamy, Selvakumar; Cheemalapati, Srikanth; Chen, Shen-Ming

    2014-01-01

    An amperometric glucose biosensor based on enhanced and fast direct electron transfer (DET) of glucose oxidase (GOx) at enzyme dispersed multiwalled carbon nanotubes/graphene oxide (MWCNT/GO) hybrid biocomposite was developed. The fabricated hybrid biocomposite was characterized by transmission electron microscopy (TEM), Raman and infrared spectroscopy (IR). The TEM image of hybrid biocomposite reveals that a thin layer of GOx was covered on the surface of MWCNT/GO hybrid composite. IR results validate that the hybrid biocomposite was formed through the electrostatic interactions between GOx and MWCNT/GO hybrid composite. Further, MWCNT/GO hybrid composite has also been characterized by TEM and UV-visible spectroscopy. A pair of well-defined redox peak was observed for GOx immobilized at the hybrid biocomposite electrode than that immobilized at the MWCNT modified electrode. The electron transfer rate constant (Ks) of GOx at the hybrid biocomposite was calculated to be 11.22s(-1). The higher Ks value revealed that fast DET of GOx occurred at the electrode surface. Moreover, fabricated biosensor showed a good sensitivity towards glucose oxidation over a linear range 0.05-23.2mM. The limit of detection (LOD) was estimated to be 28μM. The good features of the proposed biosensor could be used for the accurate detection of glucose in the biological samples. © 2013.

  19. Amperometric sensing of anti-HIV drug zidovudine on Ag nanofilm-multiwalled carbon nanotubes modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Rafati, Amir Abbas, E-mail: aa_rafati@basu.ac.ir; Afraz, Ahmadreza

    2014-06-01

    The zidovudine (ZDV) is the first drug approved for the treatment of HIV virus infection. The detection and determination of this drug are very importance in human serum because of its undesirable effects. A new ZDV sensor was fabricated on the basis of nanocomposite of silver nanofilm (Ag-NF) and multiwalled carbon nanotubes (MWCNTs) immobilized on glassy carbon electrode (GCE). The modified electrodes were characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), cyclic voltammetry (CV), and linear sweep voltammetry (LSV) techniques. Results showed that the electrodeposited silver has a nanofilm structure and further electrochemical studies showed that the prepared nanocomposite has high electrocatalytic activity and is appropriate for using in sensors. The amperometric technique under optimal conditions is used for the determination of ZDV ranging from 0.1 to 400 ppm (0.37 μM–1.5 mM) with a low detection limit of 0.04 ppm (0.15 μM) (S/N = 3) and good sensitivity. The prepared sensor possessed accurate and rapid response to ZDV and shows an average recovery of 98.6% in real samples. - Highlights: • New anti-HIV drug sensor was fabricated on the basis of nanomaterials composite. • The GCE modified by prepared hydrophilic MWCNT silver nanoparticles. • Silver nanofilm electrodeposited on MWCNT/GCE and characterized by SEM, EDX, CV and LSV • Response of electrode to ZDV was thoroughly investigated by electrochemical techniques.

  20. A sensitive label–free amperometric immunosensor for alpha-fetoprotein based on gold nanorods with different aspect ratio

    Science.gov (United States)

    Zhou, Chunyang; Liu, Dali; Xu, Lin; Li, Qingling; Song, Jian; Xu, Sai; Xing, Ruiqing; Song, Hongwei

    2015-01-01

    A simple and accurate label–free amperometric immunosensor for α–fetoprotein (AFP) detection is developed based on gold nanorods (GNRs) with different aspect ratio and compared with gold particles (GNPs). The positively charged GNRs and GNPs due to the surface immobilized cetyltrimethyl ammonium bromide (CTAB) can adsorb the negatively charged AFP antibody (Ab) directly. The presence of the GNRs not only enhanced the immobilized amount of biomolecules, but also improved the electrochemical properties of the immunosensor. With the aid of GNRs, the electrochemical signal was greatly enhanced in comparison with GNPs. Under optimal conditions, the proposed immunosensor could detect AFP in a linear range from 0.1 to 200 ng/mL with a detection limit of 0.04 ng/mL (signal–to–noise ratio = 3), and it also possessed good reproducibility and storage stability. Moreover, the detection of AFP in five human serum samples also showed satisfactory accuracy. The proposed methodology was potentially attractive for clinical immunoassay. PMID:25909588

  1. An Amperometric Immunosensor Based on Multi-Walled Carbon Nanotubes-Thionine-Chitosan Nanocomposite Film for Chlorpyrifos Detection

    Science.gov (United States)

    Sun, Xia; Cao, Yaoyao; Gong, Zhili; Wang, Xiangyou; Zhang, Yan; Gao, Jinmei

    2012-01-01

    In this work, a novel amperometric immunosensor based on multi-walled carbon nanotubes-thionine-chitosan (MWCNTs-THI-CHIT) nanocomposite film as electrode modified material was developed for the detection of chlorpyrifos residues. The nanocomposite film was dropped onto a glassy carbon electrode (GCE), and then the anti-chlorpyrifos monoclonal antibody was covalently immobilized onto the surface of MWCNTs-THI-CHIT/GCE using the crosslinking agent glutaraldehyde (GA). The modification procedure was characterized by using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Under the optimized conditions, a linear relationship between the relative change in peak current of different pulse voltammetry (DPV) and the logarithm of chlorpyrifos solution concentration was obtained in the range from 0.1 to 1.0 × 105 ng/mL with a detection limit of 0.046 ng/mL. The proposed chlorpyrifos immunosensor exhibited high reproducibility, stability, and good selectivity and regeneration, making it a potential alternative tool for ultrasensitive detection of chlorpyrifos residues in vegetables and fruits. PMID:23443396

  2. Indirect amperometric sensing of dopamine using a redox-switchable naphthoquinone-terminated self-assembled monolayer on gold electrode

    International Nuclear Information System (INIS)

    Hammami, Asma; Raouafi, Noureddine; Sahli, Rihab

    2016-01-01

    We report on the design of a simple yet sensitive and selective electrode for amperometric determination of dopamine at a cathodic potential as low as −0.30 V vs. Ag/AgCl. The electrode was obtained by self-assembly of ω-mercaptopropyl naphthoquinone (NQ-SAM) on the surface of a polycrystalline gold electrode. The presence of dopamine induces an increase of the reduction current peak at −0.30 V corresponding to the reduction of naphthoquinone to hydronaphthoquinone. Dopamine and dopamine-quinone accumulate on the surface to form a 3D network linked by hydrogen bonds. Raman and infrared spectroscopy as well as atomic force microscopy confirmed the multilayer formation. The method allows dopamine to be indirectly detected at a working potential that is lower by 0.50 V than the standard oxidation potential at a bare gold electrode. The sensor shows distinct oxidation potentials for dopamine (120 mV), ascorbic acid (280 mV) and uric acid (520 mV) which makes the method fairly selective. The analytical range extends from 1 to 100 μM concentrations of dopamine, and the limits of detection and quantification are 0.040 and 0.134 μM, respectively. (author)

  3. Amperometric Microsensors Monitoring Glutamate-Evoked In Situ Responses of Nitric Oxide and Carbon Monoxide from Live Human Neuroblastoma Cells

    Directory of Open Access Journals (Sweden)

    Yejin Ha

    2017-07-01

    Full Text Available In the brain, nitric oxide (NO and carbon monoxide (CO are important signaling gases which have multifaceted roles, such as neurotransmitters, neuromodulators, and vasodilators. Even though it is difficult to measure NO and CO in a living system due to their high diffusibility and extremely low release levels, electrochemical sensors are promising tools to measure in vivo and in vitro NO and CO gases. In this paper, using amperometric dual and septuple NO/CO microsensors, real-time NO and CO changes evoked by glutamate were monitored simultaneously for human neuroblastoma (SH-SY5Y cells. In cultures, the cells were differentiated and matured into functional neurons by retinoic acid and brain-derived neurotrophic factor. When glutamate was administrated to the cells, both NO and CO increases and subsequent decreases returning to the basal levels were observed with a dual NO/CO microsensor. In order to facilitate sensor’s measurement, a flower-type septuple NO/CO microsensor was newly developed and confirmed in terms of the sensitivity and selectivity. The septuple microsensor was employed for the measurements of NO and CO changes as a function of distances from the position of glutamate injection. Our sensor measurements revealed that only functionally differentiated cells responded to glutamate and released NO and CO.

  4. Novel amperometric sensor using metolcarb-imprinted film as the recognition element on a gold electrode and its application

    International Nuclear Information System (INIS)

    Pan Mingfei; Fang Guozhen; Liu Bing; Qian Kun; Wang Shuo

    2011-01-01

    A molecularly imprinted film is electrochemically synthesized on a gold electrode using cyclic voltammetry to electropolymerize o-aminothiophenol in the presence of metolcarb (MTMC). The mechanism of the imprinting process and a number of factors affecting the activity of the imprinted film are discussed and optimized. Scanning electron microscope observations and binding measurements have proved that an MTMC-imprinted film (with a thickness of nearly 100 nm) was formed on the surface of the gold electrode. The film exhibited high binding affinity and selectivity towards the template MTMC, as well as good penetrability, reproducibility and stability. A novel amperometry sensor using the imprinted film as recognition element was developed for MTMC determination in food samples. Under the experimental conditions, the MTMC standard is linear within the concentration range studied (r 2 = 0.9906). The limit of detection (S/N = 3) of the modified electrode was achieved to 1.34 x 10 -8 mol L -1 . Recoveries of MTMC from spiked apple juice, cabbage and cucumber samples for the developed electrochemical assay ranged from 94.80% to 102.43%, which was with great correlation coefficient (0.9929) with results from high-performance liquid chromatography. In practical application, the prepared amperometric sensor also showed good reproducibility and long lifetime for storage. The research in this study has offered a rapid, accurate and sensitive electrochemical method for quantitative determination of MTMC in food products.

  5. Amperometric biosensor for hydrogen peroxide based on Hemoglobin/DNA/Poly-2,6-pyridinediamine modified gold electrode

    International Nuclear Information System (INIS)

    Tong Zhongqiang; Yuan Ruo; Chai Yaqin; Chen Shihong; Xie Yi

    2007-01-01

    An amperometric biosensor for hydrogen peroxide (H 2 O 2 ) was fabricated based on immobilization of hemoglobin (Hb) on DNA/Poly-2,6-pyridinediamine (PPD) modified Au electrode. PPD thin films were firstly electro-deposited on Au electrode surface which provide a template to attach negatively charged DNA molecules by electrostatic attraction. The adsorbed DNA network provides a good microenvironment for the immobilization of biomolecules and promotes electron transfer between the immobilized Hb and the electrode surface. The fabrication process of the biosensor was characterized by electrochemical impedance spectroscopy. Experimental conditions influencing the biosensor performance such as pH, potential and temperature were assessed and optimized. The proposed biosensor displayed a good electrocatalytic response to the reduction of H 2 O 2 , its linear range is 1.7 μM to 3 mM with a detection limit of 1.0 μM based on the signal-to-noise ratio of 3 (S/N = 3) under the optimized conditions. The Michaelis-Menten constant K m app of Hb immobilized on the electrode surface was found to be 0.8 mM. The biosensor shows high sensitivity and stability. Importantly, this deposition methodology could be further developed for the immobilization of other proteins and biocompounds

  6. Layer-by-layer assemblies of chitosan/multi-wall carbon nanotubes and glucose oxidase for amperometric glucose biosensor applications

    International Nuclear Information System (INIS)

    Wu Baoyan; Hou Shihua; Yu Min; Qin Xia; Li, Sha; Chen Qiang

    2009-01-01

    A novel amperometric glucose biosensor based on multilayer films containing chitosan, multi-wall carbon nanotubes (MWCNTs) and glucose oxidase (GOD) was developed. MWCNTs were solubilized in chitosan (Chit-MWCNTs) used to interact with GOD. Poly (allylamine) (PAA) and polyvinylsulfuric acid potassium salt (PVS) were alternately deposited on the cleaned Pt electrode surface ((PVS/PAA) 3 /Pt). The (PVS/PAA) 3 /Pt electrode was alternately immersed in Chit-MWCNTs and GOD to assemble different layers of multilayer films. PBS washing was applied at the end of each assembly deposition for dissociating the weak adsorption. Micrographs of MWCNTs were obtained by scanning electron microscope, and properties of the resulting biosensors were measured by electrochemical measurements. Among the resulting biosensors, the biosensor based on eight layers of multilayer films was best. The resulting biosensor was able to efficiently monitor glucose, with the response time within 8 s, a detection limit of 21 μM estimated at a signal-to-noise ratio of 3, a linear range of 1-10 mM, the sensitivity of 0.45 μA/mM, and well stability. The study can provide a feasible simple approach on developing a new immobilization matrix for biosensors and surface functionalization

  7. Classification of Spanish white wines using their electrophoretic profiles obtained by capillary zone electrophoresis with amperometric detection.

    Science.gov (United States)

    Arribas, Alberto Sánchez; Martínez-Fernández, Marta; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2014-06-01

    A method was developed for the simultaneous detection of eight polyphenols (t-resveratrol, (+)-catechin, quercetin and p-coumaric, caffeic, sinapic, ferulic, and gallic acids) by CZE with electrochemical detection. Separation of these polyphenols was achieved within 25 min using a 200 mM borate buffer (pH 9.4) containing 10% methanol as separation electrolyte. Amperometric detection of polyphenols was carried out with a glassy carbon electrode (GCE) modified with a multiwalled carbon nanotubes (CNT) layer obtained from a dispersion of CNT in polyethylenimine. The excellent electrochemical properties of this modified electrode allowed the detection and quantification of the selected polyphenols in white wines without any pretreatment step, showing remarkable signal stability despite the presence of potential fouling substances in wine. The electrophoretic profiles of white wines, obtained using this methodology, have proven to be useful for the classification of these wines by means of chemometric multivariate techniques. Principal component analysis and discriminant analysis allowed accurate classification of wine samples on the basis of their grape varietal (verdejo and airén) using the information contained in selected zones of the electropherogram. The utility of the proposed CZE methodology based on the electrochemical response of CNT-modified electrodes appears to be promising in the field of wine industry and it is expected to be successfully extended to classification of a wider range of wines made of other grape varietals. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Analysis of polyphenols in white wine by CZE with amperometric detection using carbon nanotube-modified electrodes.

    Science.gov (United States)

    Moreno, Mónica; Arribas, Alberto Sánchez; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2011-04-01

    A method for the simultaneous detection of five polyphenols (caffeic, chlorogenic, ferulic and gallic acids and (+)-catechin) by CZE with electrochemical detection was developed. Separation of these polyphenols was performed in a 100 mM borate buffer (pH 9.2) within 15 min. Under optimized separation conditions, the performance of glassy carbon (GC) electrodes modified with multiwalled carbon nanotube layer obtained from different dispersions was examined. GC electrode modified with a dispersion of multi-walled carbon nanotubes (CNT) in polyethylenimine has proven to be the most suitable CNT-based electrode for its application as amperometric detector for the CZE separation of the studied compounds. The excellent electrochemical properties of this electrode allowed the detection of the selected polyphenols at +200 mV and improved the efficiency and the resolution of their CZE separation. Limits of detection below 3.1 μM were obtained with linear ranges covering the 10⁻⁵ to 10⁻⁴  M range. The proposed method has been successfully applied for the detection (ferulic, caffeic and gallic acids and (+)-catechin) and the quantification (gallic acid and (+)-catechin) of polyphenols in two different white wines without any preconcentration step. A remarkable signal stability was observed on the electrode performance despite the presence of potential fouling substances in wine. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. An amperometric uric acid biosensor based on Bis[sulfosuccinimidyl] suberate crosslinker/3-aminopropyltriethoxysilane surface modified ITO glass electrode

    International Nuclear Information System (INIS)

    Ahuja, Tarushee; Rajesh; Kumar, Devendra; Tanwar, Vinod Kumar; Sharma, Vikash; Singh, Nahar; Biradar, Ashok M.

    2010-01-01

    A label free, amperometric uric acid biosensor is described by immobilizing enzyme uricase through a self assembled monolayer (SAM) of 3-aminopropyltriethoxysilane (APTES) using a crosslinker, Bis[sulfosuccinimidyl]suberate (BS 3 ) on an indium-tin-oxide (ITO) coated glass plate. The biosensor (uricase/BS 3 /APTES/ITO) was characterized by, scanning electron microscopy (SEM), atomic force microscopy (AFM) and electrochemical techniques. Chronoamperometric response was measured as a function of uric acid concentration in aqueous solution (pH 7.4). The biosensor shows a linear response over a concentration range of 0.05 to 0.58 mM with a sensitivity of 39.35 μA mM -1 . The response time is 50 s reaching to a 95% steady state current value and about 90% of enzyme activity is retained for about 7 weeks. These results indicate an efficient binding of enzyme with the crosslinker over the surface of APTES modified ITO glass plates, which leads to an improved sensitivity and shelf life of the biosensor.

  10. Amperometric immunosensor based on multiwalled carbon nanotubes/Prussian blue/nanogold-modified electrode for determination of α-fetoprotein.

    Science.gov (United States)

    Jiang, Wen; Yuan, Ruo; Chai, Ya-Qin; Yin, Bing

    2010-12-01

    In this article, a conspicuously simple and highly sensitive amperometric immunosensor based on the sequential electrodeposition of Prussian blue (PB) and gold nanoparticles (GNPs) on multiwalled carbon nanotube (MWCNT)-modified glassy carbon electrode (GCE) surface is proposed for the detection of α-fetoprotein (AFP). By comparison with PB, the MWCNT/PB composite film had been proven to show much better electrochemical stability and a larger response current. The electrodeposited GNP film can be used not only to immobilize biomolecules but also to avoid the leakage of PB and to prevent shedding of MWCNT/PB composite film from the electrode surface. The performance and factors influencing the performance of the immunosensor were investigated. Under optimal experimental conditions, the proposed immunosensor for AFP was observed with an ultralow limit of detection (LOD) equal to 3 pg/ml (at 3δ), and the linear working range spanned the concentrations of AFP from 0.01 to 300 ng/ml. Moreover, the immunosensor, as well as a commercially available kit, was examined for use in the determination of AFP in real human serum specimens. More significant, the assay mentioned here is simpler than the traditional enzyme-linked immunosorbent assay (ELISA), and an excellent correlation of levels of AFP measured was obtained, indicating that the developed immunoassay could be a promising alternative approach for detection of AFP and other tumor markers in the clinical diagnosis. Copyright © 2010 Elsevier Inc. All rights reserved.

  11. Direct electrodeposition of highly ordered gold nanotube arrays for use in non-enzymatic amperometric sensing of glucose

    International Nuclear Information System (INIS)

    Tian, Taolei; Dong, Junping; Xu, Jiaqiang

    2016-01-01

    The authors describe vertically aligned gold nanotube arrays (Au-NTAs) and gold nanowire arrays (Au-NWAs) that were directly grown in alumina oxide templates by galvanostatic deposition. The morphology of the gold arrays can be controlled by adjusting the pH value of the plating bath. Scanning electron microscopy shows the nanoarrays to be highly ordered (with an average length of around 2 μm), and the opening width of the gold nanotube arrays to be uniform (with diameters of around 50 nm). The electrocatalytic activities of the Au-NTAs and Au-NWAs deposited on a glassy carbon electrode toward glucose oxidation were compared by cyclic voltammetry and amperometry at pH 7.2. The Au-NTAs yield higher amperometric currents. The respective glucose sensor, when operated at a working potential of 0.25 V (vs. SCE), exhibits a linear range that extends from 5 μM to 16.4 mM concentrations of glucose, a sensitivity of 44.2 μA mM"−"1 cm"−"2, and a detection limit of 2.1 μM (at an S/N ratio of 3). The excellent sensing performance is attributed to the large surface area and the fast electron transfer rate for the one-dimensional gold nanoarrays (author)

  12. Novel amperometric sensor using metolcarb-imprinted film as the recognition element on a gold electrode and its application

    Energy Technology Data Exchange (ETDEWEB)

    Pan Mingfei; Fang Guozhen; Liu Bing; Qian Kun [Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457 (China); Wang Shuo, E-mail: pmf2006@126.com [Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin 300457 (China)

    2011-04-01

    A molecularly imprinted film is electrochemically synthesized on a gold electrode using cyclic voltammetry to electropolymerize o-aminothiophenol in the presence of metolcarb (MTMC). The mechanism of the imprinting process and a number of factors affecting the activity of the imprinted film are discussed and optimized. Scanning electron microscope observations and binding measurements have proved that an MTMC-imprinted film (with a thickness of nearly 100 nm) was formed on the surface of the gold electrode. The film exhibited high binding affinity and selectivity towards the template MTMC, as well as good penetrability, reproducibility and stability. A novel amperometry sensor using the imprinted film as recognition element was developed for MTMC determination in food samples. Under the experimental conditions, the MTMC standard is linear within the concentration range studied (r{sup 2} = 0.9906). The limit of detection (S/N = 3) of the modified electrode was achieved to 1.34 x 10{sup -8} mol L{sup -1}. Recoveries of MTMC from spiked apple juice, cabbage and cucumber samples for the developed electrochemical assay ranged from 94.80% to 102.43%, which was with great correlation coefficient (0.9929) with results from high-performance liquid chromatography. In practical application, the prepared amperometric sensor also showed good reproducibility and long lifetime for storage. The research in this study has offered a rapid, accurate and sensitive electrochemical method for quantitative determination of MTMC in food products.

  13. Carbon Fiber Ultramicrodic Electrode Electrodeposited with Over-Oxidized Polypyrrole for Amperometric Detection of Vesicular Exocytosis from Pheochromocytoma Cell

    Directory of Open Access Journals (Sweden)

    Li Wang

    2015-01-01

    Full Text Available Vesicular exocytosis is ubiquitous, but it is difficult to detect within the cells’ communication mechanism. For this purpose, a 2 µm ultramicrodic carbon fiber electrode was fabricated in this work based on electrodeposition with over-oxidized polypyrrole nanoparticle (PPyox-CFE, which was applied successfully for real-time monitoring of quantal exocytosis from individual pheochromocytoma (PC12 cells. PPyox-CFE was evaluated by dopamine (DA solutions through cyclic voltammetry and amperometry electrochemical methods, and results revealed that PPyox-CFE improved the detection limit of DA. In particular, the sensitivity of DA was improved to 24.55 µA·µM−1·µm−2 using the PPyox-CFE. The ultramicrodic electrode combined with the patch-clamp system was used to detect vesicular exocytosis of DA from individual PC12 cells with 60 mM K+ stimulation. A total of 287 spikes released from 7 PC12 cells were statistically analyzed. The current amplitude (Imax and the released charge (Q of the amperometric spikes from the DA release by a stimulated PC12 cell is 45.1 ± 12.5 pA and 0.18 ± 0.04 pC, respectively. Furthermore, on average ~562,000 molecules were released in each vesicular exocytosis. PPyox-CFE, with its capability of detecting vesicular exocytosis, has potential application in neuron communication research.

  14. Amperometric detection of carbohydrates based on the glassy carbon electrode modified with gold nano-flake layer

    Directory of Open Access Journals (Sweden)

    Huy Du Nguyen

    2015-09-01

    Full Text Available An electro-deposition approach was established to incorporate the gold nano-flakes onto the glassy carbon electrode in electrochemical cells (nano-Au/GC/ECCs. Using pulsed amperometric detection (PAD without any gold oxidation for cleaning (non-oxidative PAD, the nano-Au/GC/ECCs were able to maintain their activity for oxidizing of carbohydrates in a normal alkaline medium. The reproducibility of peak area was about 2 relative standard deviation (RSD,% for 6 consecutive injections. A dynamic range of carbohydrates was obtained over a concentration range of 5–80 mg L−1 and the limits of detection (LOD were of 2 mg L−1 for fructose and lactose and 1 mg L−1 for glucose and galactose. Moreover, the nano-Au/GC/ECC using the non-oxidative PAD was able to combine with the internal standard method for determination of lactose in fresh cow milk sample.

  15. Simultaneous Determination of the Main Peanut Allergens in Foods Using Disposable Amperometric Magnetic Beads-Based Immunosensing Platforms

    Directory of Open Access Journals (Sweden)

    Víctor Ruiz-Valdepeñas Montiel

    2016-06-01

    Full Text Available In this work, a novel magnetic beads (MBs-based immunosensing approach for the rapid and simultaneous determination of the main peanut allergenic proteins (Ara h 1 and Ara h 2 is reported. It involves the use of sandwich-type immunoassays using selective capture and detector antibodies and carboxylic acid-modified magnetic beads (HOOC-MBs. Amperometric detection at −0.20 V was performed using dual screen-printed carbon electrodes (SPdCEs and the H2O2/hydroquinone (HQ system. This methodology exhibits high sensitivity and selectivity for the target proteins providing detection limits of 18.0 and 0.07 ng/mL for Ara h 1 and Ara h 2, respectively, with an assay time of only 2 h. The usefulness of the approach was evaluated by detecting the endogenous content of both allergenic proteins in different food extracts as well as trace amounts of peanut allergen (0.0001% or 1.0 mg/kg in wheat flour spiked samples. The developed platform provides better Low detection limits (LODs in shorter assay times than those claimed for the allergen specific commercial ELISA kits using the same immunoreagents and quantitative information on individual food allergen levels. Moreover, the flexibility of the methodology makes it readily translate to the detection of other food-allergens.

  16. Amperometric inhibition biosensors based on horseradish peroxidase and gold sononanoparticles immobilized onto different electrodes for cyanide measurements.

    Science.gov (United States)

    Attar, Aisha; Cubillana-Aguilera, Laura; Naranjo-Rodríguez, Ignacio; de Cisneros, José Luis Hidalgo-Hidalgo; Palacios-Santander, José María; Amine, Aziz

    2015-02-01

    New biosensors based on inhibition for the detection of cyanide and the comparison of the analytical performances of nine enzyme biosensor designs by using three different electrodes: Sonogel-Carbon, glassy carbon and gold electrodes were discussed. Three different horseradish peroxidase immobilization procedures with and without gold sononanoparticles were studied. The amperometric measurements were performed at an applied potential of -0.15V vs. Ag/AgCl in 50mM sodium acetate buffer solution pH=5.0. The apparent kinetic parameters (Kmapp, Vmaxapp) of immobilized HRP were calculated in the absence of inhibitor (cyanide) by using caffeic acid, hydroquinone, and catechol as substrates. The presence of gold sononanoparticles enhanced the electron transfer reaction and improved the analytical performance of the biosensors. The HRP kinetic interactions reveal non-competitive binding of cyanide with an apparent inhibition constant (Ki) of 2.7μM and I50 of 1.3μM. The determination of cyanide can be achieved in a dynamic range of 0.1-58.6μM with a detection limit of 0.03μM which is lower than those reported by previous studies. Hence this biosensing methodology can be used as a new promising approach for detecting cyanide. Copyright © 2014. Published by Elsevier B.V.

  17. Rhodium-Prussian Blue modified carbon paste electrode (Rh-PBMCPE for amperometric detection of hydrogen peroxide

    Directory of Open Access Journals (Sweden)

    Ivama Viviane Midori

    2003-01-01

    Full Text Available Prussian Blue was deposited at carbon paste electrode surface from a solution containing 2.0 x 10-3 mol L-1 K3[Fe(CN6], 3.0 x 10-3 mol L-1 FeCl3 and 1.0 x 10-2 mol L-1 HCl using two controlled potentials. To improve the stability of the modified electrode it was 50 times cycled in a solution containing 1.0 x 10-3 mol L-1 RhCl3, 0.50 mol L-1 KCl and 0.010 mol L-1 HCl in the potential range from - 0.40 V to 0.60 V at 60 mV s-1. The Rh - Prussian Blue carbon paste modified electrode (Rh-PBMCPE showed good stability during amperometric catalytic determination of H2O2 at 0.040 V, without ascorbic and uric acids interferences. The current changed linearly with H2O2 concentrations in the range of 5.0 x 10-5 - 8.6 x 10-4 mol L-1. The estimated detection limit was 2.8 x 10-5 mol L-1 with sensibility changing from 1.32 to 0.96 A mol-1 L cm-2 along five days (180 determinations.

  18. Amperometric catechol biosensor based on laccase immobilized on nitrogen-doped ordered mesoporous carbon (N-OMC)/PVA matrix

    International Nuclear Information System (INIS)

    Guo, Meiqing; Wang, Hefeng; Huang, Di; Han, Zhijun; Wang, Xiaojun; Li, Qiang; Chen, Jing

    2014-01-01

    A functionalized nitrogen-containing ordered mesoporous carbon (N-OMC), which shows good electrical properties, was synthesized by the carbonization of polyaniline inside a SBA-15 mesoporous silica template. Based on this, through entrapping laccase onto the N-OMC/polyvinyl alcohol (PVA) film a facilely fabricated amperometric biosensor was developed. Laccase from Trametes versicolor was assembled on a composite film of a N-OMC/PVA modified Au electrode and the electrochemical behavior was investigated. The results indicated that the N-OMC modified electrode exhibits electrical properties towards catechol. The optimum experimental conditions of a biosensor for the detection of catechol were studied in detail. Under the optimal conditions, the sensitivity of the biosensor was 0.29 A*M −1 with a detection limit of 0.31 μM and a linear detection range from 0.39 μM to 8.98 μM for catechol. The calibration curve followed the Michaelis–Menten kinetics and the apparent Michaelis–Menten (K M app ) was 6.28 μM. This work demonstrated that the N-OMC/PVA composite provides a suitable support for laccase immobilization and the construction of a biosensor. (papers)

  19. Detection of Waterborne and Airborne Formaldehyde: From Amperometric Chemosensing to a Visual Biosensor Based on Alcohol Oxidase

    Directory of Open Access Journals (Sweden)

    Sasi Sigawi

    2014-02-01

    Full Text Available A laboratory prototype of a microcomputer-based analyzer was developed for quantitative determination of formaldehyde in liquid samples, based on catalytic chemosensing elements. It was shown that selectivity for the target analyte could be increased by modulating the working electrode potential. Analytical parameters of three variants of the amperometric analyzer that differed in the chemical structure/configuration of the working electrode were studied. The constructed analyzer was tested on wastewater solutions that contained formaldehyde. A simple low-cost biosensor was developed for semi-quantitative detection of airborne formaldehyde in concentrations exceeding the threshold level. This biosensor is based on a change in the color of a solution that contains a mixture of alcohol oxidase from the yeast Hansenula polymorpha, horseradish peroxidase and a chromogen, following exposure to airborne formaldehyde. The solution is enclosed within a membrane device, which is permeable to formaldehyde vapors. The most efficient and sensitive biosensor for detecting formaldehyde was the one that contained alcohol oxidase with an activity of 1.2 U·mL−1. The biosensor requires no special instrumentation and enables rapid visual detection of airborne formaldehyde at concentrations, which are hazardous to human health.

  20. Determination of sugar compounds in olive plant extracts by anion-exchange chromatography with pulsed amperometric detection.

    Science.gov (United States)

    Cataldi, T R; Margiotta, G; Iasi, L; Di Chio, B; Xiloyannis, C; Bufo, S A

    2000-08-15

    We describe a chromatographic method that uses isocratic elution and pulsed amperometric detection to determine soluble carbohydrates in plant tissues. Such a method provides a rapid and convenient means to obtain a complete profile of the sugar components of leaves and roots from olive (Olea europaea L. cv. Coratina) plants. A simple purification of plant extracts using pure water was developed, which is far less time-consuming and retains a high level of accuracy. Excellent separation of myo-inositol, galactinol, mannitol, galactose, glucose, fructose, sucrose, raffinose, and stachyose was achieved with an anion-exchange column and 12 mM NaOH spiked with 1 mM barium acetate as an eluent. At a flow rate of 1.0 mL/min, the time of analysis was less than 25 min, and repeatability of the method on the order of 2.2% as RSD or better for retention times and lower than 5.2% for peak areas. Recoveries approximated 100% (range 97.2-104.5%), and the method provided good precision with a coefficient of variation which ranged between 0.9 and 3.3%. Among identified carbohydrates extracted from leaves and roots of olive plants, glucose and mannitol were major compounds. Their molar ratio was estimated to be 1.2+/-0.1 and 2.2+/-0.3 for olive leaves and roots, respectively. The occurrence of soluble galactinol in plant tissues was also validated.

  1. Amperometric cholesterol biosensor based on in situ reconstituted cholesterol oxidase on an immobilized monolayer of flavin adenine dinucleotide cofactor.

    Science.gov (United States)

    Vidal, Juan-C; Espuelas, Javier; Castillo, Juan-R

    2004-10-01

    A new amperometric biosensor for determining cholesterol based on deflavination of the enzyme cholesterol oxidase (ChOx) and subsequent reconstitution of the apo-protein with a complexed flavin adenine dinucleotide (FAD) monolayer is described. The charge transfer mediator pyrroquinoline quinone (PQQ) was covalently bound to a cystamine self-assembled monolayer (SAM) on an Au electrode. Boronic acid (BA) was then bound to PQQ using the carbodiimide procedure, and the BA ligand was complexed to the FAD molecules on which the apo-ChOx was subsequently reconstituted. The effective release of the FAD from the enzyme and the successful reconstitution were verified using molecular fluorescence and cyclic voltammetry. The optimal orientation of FAD toward the PQQ mediator and the distances between FAD and PQQ and between PQQ and electrode enhance the charge transfer, very high sensitivity (about 2,500 nAmM(-1)cm(-2)) being obtained for cholesterol determination. The biosensor is selective toward electroactive interferents (ascorbic acid and uric acid) and was tested in reference serum samples, demonstrating excellent accuracy (relative errors below 3% in all cases). The biosensor activity can be successfully regenerated in a simple process by successive reconstitution with batches of recently prepared apo-ChOx on the same immobilized Au/SAM-PQQ-BA-FAD monolayer (it was tested five times); the lifetime of the biosensor is about 45-60 days.

  2. Preparation of carbon paste electrodes including poly(styrene) attached glycine-Pt(IV) for amperometric detection of glucose.

    Science.gov (United States)

    Dönmez, Soner; Arslan, Fatma; Sarı, Nurşen; Kurnaz Yetim, Nurdan; Arslan, Halit

    2014-04-15

    In this study, a novel carbon paste electrode that is sensitive to glucose was prepared using the nanoparticles modified (4-Formyl-3-methoxyphenoxymethyl) with polystyren (FMPS) with L-Glycine-Pt(IV) complexes. Polymeric nanoparticles having Pt(IV) ion were prepared from (4-Formyl-3-methoxyphenoxymethyl) polystyren, glycine and PtCl4 by template method. Glucose oxidase enzyme was immobilized to a modified carbon paste electrode (MCPE) by cross-linking with glutaraldehyde. Determination of glucose was carried out by oxidation of enzymatically produced H2O2 at 0.5 V vs. Ag/AgCl. Effects of pH and temperature were investigated, and optimum parameters were found to be 8.0 and 55°C, respectively. Linear working range of the electrode was 5.0×10(-6)-1.0×10(-3) M, R(2)=0.997. Storage stability and operational stability of the enzyme electrode were also studied. Glucose biosensor gave perfect reproducible results after 10 measurements with 2.3% relative standard deviation. Also, it had good storage stability (gave 53.57% of the initial amperometric response at the end of 33th day). © 2013 Published by Elsevier B.V.

  3. Determinação espectrofotométrica de vitamina B2 (riboflavina) em formulações farmacêuticas empregando sistema de análises por injeção em fluxo Spectrophotometric determination of vitamin B2 (riboflavin) in pharmaceutical formulations using flow injection analysis

    OpenAIRE

    Clezio Aniceto; Larissa de Souza Canaes; Orlando Fatibello-Filho; Carla C. S. Cavalheiro

    2000-01-01

    A flow injection spectrophotometric procedure exploiting merging zones is proposed for determining vitamin B2 (riboflavin) in pharmaceutical preparations. The determination is based on the red-colored complex formation between vitamin B2 and silver(I) which was measured at 520 nm. Vitamin B2 was determined in four pharmaceutical preparations in the 1.0 to 50.0 mg L-1 concentration range, with a detection limit of 0.5 mg L-1. The recovery from three samples ranged from 98.0 to 104.0 %. The ana...

  4. An amperometric enzyme electrode and its biofuel cell based on a glucose oxidase-poly(3-anilineboronic acid)-Pd nanoparticles bionanocomposite for glucose biosensing.

    Science.gov (United States)

    Sun, Lingen; Ma, Yixuan; Zhang, Pei; Chao, Long; Huang, Ting; Xie, Qingji; Chen, Chao; Yao, Shouzhuo

    2015-06-01

    A new amperometric enzyme electrode and its biofuel cell were fabricated based on a glucose oxidase (GOx)-poly(3-anilineboronic acid) (PABA)-Pd nanoparticles (PdNPs) bionanocomposite for biosensing of glucose. Briefly, Pd was electroplated on a multiwalled carbon nanotubes (MWCNTs)-modified Au electrode, and the GOx-PABA-PdNPs bionanocomposite was prepared on the Pd(plate)/MWCNTs/Au electrode through the chemical oxidation of a GOx-3-anilineboronic acid adduct by Na2PdCl4, followed by electrode-modification with an outer-layer chitosan (CS) film. The thus-prepared CS/GOx-PABA-PdNPs/Pd(plate)/MWCNTs/Au electrode exhibited a linear amperometric response to glucose concentration from 2.0 μM to 4.5 mM with a sensitivity of 160 μA/mM/cm(2), sub-μM detection limit, and excellent operation/storage stability in the first-generation biosensing mode, as well as excellent analytical performance in the second-generation biosensing mode. The good recoveries of glucose obtained from spiked urine samples revealed the application potential of our amperometric enzyme electrode. In addition, a glucose/O2 biofuel cell was constructed using this enzyme electrode as the anode and a Pt/MWCNTs/Au electrode as the cathode, and this biofuel cell as a self-powered biosensing device showed a linear voltage response to glucose concentration from 100 μM to 13.5 mM with a sensitivity of 43.5 mV/mM/cm(2) and excellent operation/storage stability. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Enhanced amperometric response of a glucose oxidase and horseradish peroxidase based bienzyme glucose biosensor modified with a film of polymerized toluidine blue containing reduced graphene oxide

    International Nuclear Information System (INIS)

    Wang, Fang; Gong, Wencheng; Wang, Lili; Chen, Zilin

    2015-01-01

    Reduced graphene oxide (RGO) was used to construct a bienzyme biosensor containing horseradish peroxidase (HRP) and glucose oxidase (GOx). A poly(toluidine blue) (pTB) film containing RGO acted as both enzyme immobilization matrix and electron transfer mediator. The bienzyme biosensor was characterized by electrochemical techniques and displays a highly sensitive amperometric response to glucose and hydrogen peroxide (H 2 O 2 ) at a potential as low as −0.1 V (vs. SCE). It is shown that use of RGO causes a strong enhancement on the amperometric responses. H 2 O 2 formed by the action of GOx in the presence of oxygen can be further reduced by HRP in the pTB film contacting the RGO modified electrode. In the absence of oxygen, glucose oxidation proceeds by another mechanism in which electron transfer occurs from GOx to the electrode and with pTB acting as the mediator. Amperometric responses to glucose and H2O2 follow Michaelis-Menten kinetics. The experimental conditions were optimized, and under these conditions glucose can be determined in the 80 μM to 3.0 mM range with a detection limit of 50 μM. H 2 O 2 , in turn, can be quantified in up to 30.0 μM concentration with a detection limit of 0.2 μM. The bienzyme biosensor is reproducible, repeatable and stable. Finally, it has been successfully applied to the determination of glucose in plasma samples. (author)

  6. Development of a novel biosensor based on a polypyrrole-dodecylbenzene sulphonate (PPy-DBS) film for the determination of amperometric cholesterol.

    Science.gov (United States)

    Özer, Bayram Oğuz; Çete, Servet

    2017-06-01

    Herein a novel amperometric biosensor based on a conducting polymer with anionic dopant modified electrode was successfully developed for detection of cholesterol. Polypyrrole is deposited on a platinum surface and the sodium dodecylbenzene sulphonate (DBS) ion-doped polypyrrole film was electrochemically prepared by scanning the electrode potential between -0.8 and +0.8 V at a scan rate of 20 mV/s. The present electrochemical biosensor was optimized in terms of working potential, number of cycles, concentrations of monomer, and anionic dopant. Cholesterol oxidase (ChOx) was physically entrapped in PPy-DBS to construct an amperometric cholesterol biosensor. Amperometric determination is based on the electrochemical detection of H 2 O 2 generated in the enzymatic reaction of cholesterol. Kinetic parameters, operational and storage stabilities, pH, and temperature dependencies were determined. Km and Imax were calculated as 0.11 μM and 0.967 nM/min, respectively. The operational stability results showed that 90.0% of the response current was retained after 30 activity assays. Morphology of electrodes was characterized by SEM and AFM. Additionally, contact angle measurements were made with 1 μL water of polymer film and enzyme electrode. As a result, the cholesterol biosensor suggested in this study is easy to prepare and is highly cost-effective. This composite (PPy-DBS) can supply a biocompatible and electrochemical microenvironment for immobilization of the enzyme, making this material a good candidate for the fabrication of highly sensitive and selective cholesterol biosensors.

  7. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

    OpenAIRE

    Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

    2017-01-01

    A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detec...

  8. Detection and quantification of new psychoactive substances (NPSs) within the evolved "legal high" product, NRG-2, using high performance liquid chromatography-amperometric detection (HPLC-AD).

    Science.gov (United States)

    Zuway, Khaled Y; Smith, Jamie P; Foster, Christopher W; Kapur, Nikil; Banks, Craig E; Sutcliffe, Oliver B

    2015-09-21

    The global increase in the production and abuse of cathinone-derived New Psychoactive Substances (NPSs) has developed the requirement for rapid, selective and sensitive protocols for their separation and detection. Electrochemical sensing of these compounds has been demonstrated to be an effective method for the in-field detection of these substances, either in their pure form or in the presence of common adulterants, however, the technique is limited in its ability to discriminate between structurally related cathinone-derivatives (for example: (±)-4′-methylmethcathinone (4-MMC, 2a) and (±)-4′-methyl-N-ethylmethcathinone (4-MEC, 2b) when they are both present in a mixture. In this paper we demonstrate, for the first time, the combination of HPLC-UV with amperometric detection (HPLC-AD) for the qualitative and quantitative analysis of 4-MMC and 4-MEC using either a commercially available impinging jet (LC-FC-A) or custom-made iCell channel (LC-FC-B) flow-cell system incorporating embedded graphite screen-printed macroelectrodes. The protocol offers a cost-effective, reproducible and reliable sensor platform for the simultaneous HPLC-UV and amperometric detection of the target analytes. The two systems have similar limits of detection, in terms of amperometric detection [LC-FC-A: 14.66 μg mL(-1) (2a) and 9.35 μg mL(-1) (2b); LC-FC-B: 57.92 μg mL(-1) (2a) and 26.91 μg mL(-1) (2b)], to the previously reported oxidative electrochemical protocol [39.8 μg mL(-1) (2a) and 84.2 μg mL(-1) (2b)], for two synthetic cathinones, prevalent on the recreational drugs market. Though not as sensitive as standard HPLC-UV detection, both flow cells show a good agreement, between the quantitative electroanalytical data, thereby making them suitable for the detection and quantification of 4-MMC and 4-MEC, either in their pure form or within complex mixtures. Additionally, the simultaneous HPLC-UV and amperometric detection protocol detailed herein shows a marked improvement

  9. A highly sensitive hydrogen peroxide amperometric sensor based on MnO2-modified vertically aligned multiwalled carbon nanotubes.

    Science.gov (United States)

    Xu, Bin; Ye, Min-Ling; Yu, Yu-Xiang; Zhang, Wei-De

    2010-07-26

    In this report, a highly sensitive amperometric sensor based on MnO(2)-modified vertically aligned multiwalled carbon nanotubes (MnO(2)/VACNTs) for determination of hydrogen peroxide (H(2)O(2)) was fabricated by electrodeposition. The morphology of the nanocomposite was characterized by scanning electron microscopy, energy-dispersive X-ray spectrometer and X-ray diffraction. Cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy were applied to investigate the electrochemical properties of the MnO(2)/VACNTs nanocomposite electrode. The mechanism for the electrochemical reaction of H(2)O(2) at the MnO(2)/VACNTs nanocomposite electrode was also discussed. In borate buffer (pH 7.8, 0.20 M), the MnO(2)/VACNTs nanocomposite electrode exhibits a linear dependence (R=0.998) on the concentration of H(2)O(2) from 1.2 x 10(-6)M to 1.8 x 10(-3)M, a high sensitivity of 1.08 x 10(6) microA M(-1) cm(-2) and a detection limit of 8.0 x 10(-7) M (signal/noise=3). Meanwhile, the MnO(2)/VACNTs nanocomposite electrode is also highly resistant towards typical inorganic salts and some biomolecules such as acetic acid, citric acid, uric acid and D-(+)-glucose, etc. In addition, the sensor based on the MnO(2)/VACNTs nanocomposite electrode was applied for the determination of trace of H(2)O(2) in milk with high accuracy, demonstrating its potential for practical application. Copyright 2010 Elsevier B.V. All rights reserved.

  10. Pulsed amperometric detection at glassy carbon electrodes: A new waveform for sensitive and reproducible determination of electroactive compounds.

    Science.gov (United States)

    Nardiello, Donatella; Palermo, Carmen; Natale, Anna; Quinto, Maurizio; Centonze, Diego

    2015-09-24

    In this work, the application of a new pulsed amperometric detection (PAD) waveform at a glassy carbon electrode, operating in typical chromatographic mobile phases, is proposed for the sensitive and reproducible determination of arylethanolaminic and phenolic moiety based compounds (e.g. beta-agonists and polyphenols). Preliminary experiments by cyclic voltammetry were carried out to investigate the electrochemical behaviour and to select the detection and cleaning electrode potentials. The proposed potential-time profile was designed to prevent the carbon electrode fouling under repeated analyses, thus ensuring a reproducible and sensitive quantitative determination, without the need of any mechanical or chemical electrode cleaning procedure. The waveform electrochemical parameters, including detection and delay times, were optimized in terms of sensitivity, limit of detection and response stability. The optimized waveform allowed the sensitive and stable detection of model compounds, such as clenbuterol and caffeic acid, that showed detection limits of 0.1 μg L(-1) and 14 μg L(-1), quantification limits of 0.4 μg L(-1) and 46 μg L(-1), and linearity up to 100 μg L(-1) (r = 0.9993) and 10 mg L(-1) (r = 0.9998), respectively. Similar results were obtained for other compounds of the same classes, with precision values under repeatability conditions ranging from 3.0 to 5.9%. The proposed method can be then considered as an excellent alternative to the post-column detection of beta-agonists, phenols and polyphenols. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. An amperometric hydrogen peroxide biosensor based on Co3O4 nanoparticles and multiwalled carbon nanotube modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Kaçar, Ceren; Dalkiran, Berna; Erden, Pınar Esra; Kiliç, Esma

    2014-01-01

    Highlights: • Hydrogen peroxide biosensor was constructed by combining the advantageous properties of MWCNTs and Co 3 O 4 . • Incorporating Co 3 O 4 nanoparticles into MWCNTs/gelatin film increased the electron transfer. • Co 3 O 4 /MWCNTs/gelatin/HRP/Nafion/GCE showed strong anti-interference ability. • Hydrogen peroxide was successfully determined in disinfector with an average recovery of 100.78 ± 0.89. - Abstract: In this work a new type of hydrogen peroxide biosensor was fabricated based on the immobilization of horseradish peroxidase (HRP) by cross-linking on a glassy carbon electrode (GCE) modified with Co 3 O 4 nanoparticles, multiwall carbon nanotubes (MWCNTs) and gelatin. The introduction of MWCNTs and Co 3 O 4 nanoparticles not only enhanced the surface area of the modified electrode for enzyme immobilization but also facilitated the electron transfer rate, resulting in a high sensitivity of the biosensor. The fabrication process of the sensing surface was characterized by scanning electron microscopy (SEM), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Amperometric detection of hydrogen peroxide was investigated by holding the modified electrode at −0.30 V (vs. Ag/AgCl). The biosensor showed optimum response within 5 s at pH 7.0. The optimized biosensor showed linear response range of 7.4 × 10 −7 –1.9 × 10 −5 M with a detection limit of 7.4 × 10 −7 . The applicability of the purposed biosensor was tested by detecting hydrogen peroxide in disinfector samples. The average recovery was calculated as 100.78 ± 0.89

  12. Determination of total creatine kinase activity in blood serum using an amperometric biosensor based on glucose oxidase and hexokinase.

    Science.gov (United States)

    Kucherenko, I S; Soldatkin, O O; Lagarde, F; Jaffrezic-Renault, N; Dzyadevych, S V; Soldatkin, A P

    2015-11-01

    Creatine kinase (CK: adenosine-5-triphosphate-creatine phosphotransferase) is an important enzyme of muscle cells; the presence of a large amount of the enzyme in blood serum is a biomarker of muscular injuries, such as acute myocardial infarction. This work describes a bi-enzyme (glucose oxidase and hexokinase based) biosensor for rapid and convenient determination of CK activity by measuring the rate of ATP production by this enzyme. Simultaneously the biosensor determines glucose concentration in the sample. Platinum disk electrodes were used as amperometric transducers. Glucose oxidase and hexokinase were co-immobilized via cross-linking with BSA by glutaraldehyde and served as a biorecognition element of the biosensor. The biosensor work at different concentrations of CK substrates (ADP and creatine phosphate) was investigated; optimal concentration of ADP was 1mM, and creatine phosphate - 10 mM. The reproducibility of the biosensor responses to glucose, ATP and CK during a day was tested (relative standard deviation of 15 responses to glucose was 2%, to ATP - 6%, to CK - 7-18% depending on concentration of the CK). Total time of CK analysis was 10 min. The measurements of creatine kinase in blood serum samples were carried out (at 20-fold sample dilution). Twentyfold dilution of serum samples was chosen as optimal for CK determination. The biosensor could distinguish healthy and ill people and evaluate the level of CK increase. Thus, the biosensor can be used as a test-system for CK analysis in blood serum or serve as a component of multibiosensors for determination of important blood substances. Determination of activity of other kinases by the developed biosensor is also possible for research purposes. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Layer-by-Layer Self-Assembling Gold Nanorods and Glucose Oxidase onto Carbon Nanotubes Functionalized Sol-Gel Matrix for an Amperometric Glucose Biosensor.

    Science.gov (United States)

    Wu, Baoyan; Hou, Shihua; Miao, Zhiying; Zhang, Cong; Ji, Yanhong

    2015-09-18

    A novel amperometric glucose biosensor was fabricated by layer-by-layer self-assembly of gold nanorods (AuNRs) and glucose oxidase (GOD) onto single-walled carbon nanotubes (SWCNTs)-functionalized three-dimensional sol-gel matrix. A thiolated aqueous silica sol containing SWCNTs was first assembled on the surface of a cleaned Au electrode, and then the alternate self-assembly of AuNRs and GOD were repeated to assemble multilayer films of AuNRs-GOD onto SWCNTs-functionalized silica gel for optimizing the biosensor. Among the resulting glucose biosensors, the four layers of AuNRs-GOD-modified electrode showed the best performance. The sol-SWCNTs-(AuNRs- GOD)₄/Au biosensor exhibited a good linear range of 0.01-8 mM glucose, high sensitivity of 1.08 μA/mM, and fast amperometric response within 4 s. The good performance of the proposed glucose biosensor could be mainly attributed to the advantages of the three-dimensional sol-gel matrix and stereo self-assembly films, and the natural features of one-dimensional nanostructure SWCNTs and AuNRs. This study may provide a new facile way to fabricate the enzyme-based biosensor with high performance.

  14. Determination of biogenic amines in chocolate by ion chromatographic separation and pulsed integrated amperometric detection with implemented wave-form at Au disposable electrode.

    Science.gov (United States)

    Pastore, Paolo; Favaro, Gabriella; Badocco, Denis; Tapparo, Andrea; Cavalli, Silvano; Saccani, Giovanna

    2005-12-09

    A rapid and selective cation exchange chromatographic method coupled to integrated pulsed amperometric detection (PAD) has been developed to quantify biogenic amines in chocolate. The method is based on gradient elution of aqueous methanesulfonic acid with post column addition of strong base to obtain suitable conditions for amperometric detection. A potential waveform able to keep long time performance of the Au disposable electrode was set up. Total analysis time is less than 20min. Concentration levels of dopamine, serotonin, tyramine, histamine and 2-phenylethylamine were measured, after extraction with perchloric acid from 2g samples previously defatted twice with petroleum ether. The method was used to determine the analytes in chocolate real matrices and their quantification was made with standard addition method. Only dopamine, histamine and serotonin were found in the analysed real samples. Repeatabilities of their signals, computed on their amounts in the real samples, were 5% for all of them. Repeatabilities of tyramine and phenethylamine were relative to standard additions to real samples (close to 1mg/l in the extract) and were 7 and 3%, respectively. Detection limits were computed with the 3s of the baseline noise combined with the calibration plot regression parameters. They were satisfactorily low for all amines: 3mg/kg for dopamine, 2mg/kg for tyramine, 1mg/kg for histamine, 2mg/kg for serotonin, 3mg/kg for 2-phenylethylamine.

  15. Layer-by-Layer Self-Assembling Gold Nanorods and Glucose Oxidase onto Carbon Nanotubes Functionalized Sol-Gel Matrix for an Amperometric Glucose Biosensor

    Directory of Open Access Journals (Sweden)

    Baoyan Wu

    2015-09-01

    Full Text Available A novel amperometric glucose biosensor was fabricated by layer-by-layer self-assembly of gold nanorods (AuNRs and glucose oxidase (GOD onto single-walled carbon nanotubes (SWCNTs-functionalized three-dimensional sol-gel matrix. A thiolated aqueous silica sol containing SWCNTs was first assembled on the surface of a cleaned Au electrode, and then the alternate self-assembly of AuNRs and GOD were repeated to assemble multilayer films of AuNRs-GOD onto SWCNTs-functionalized silica gel for optimizing the biosensor. Among the resulting glucose biosensors, the four layers of AuNRs-GOD-modified electrode showed the best performance. The sol-SWCNTs-(AuNRs- GOD4/Au biosensor exhibited a good linear range of 0.01–8 mM glucose, high sensitivity of 1.08 μA/mM, and fast amperometric response within 4 s. The good performance of the proposed glucose biosensor could be mainly attributed to the advantages of the three-dimensional sol-gel matrix and stereo self-assembly films, and the natural features of one-dimensional nanostructure SWCNTs and AuNRs. This study may provide a new facile way to fabricate the enzyme-based biosensor with high performance.

  16. A green synthetic strategy of nickel hexacyanoferrate nanoparticals supported on the graphene substrate and its non-enzymatic amperometric sensing application

    Energy Technology Data Exchange (ETDEWEB)

    Xue, Zhonghua, E-mail: xzh@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province, College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); He, Nan [Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province, College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Rao, Honghong [College of Chemistry and Chemical Engineering, Lanzhou City University, Lanzhou, 730070 (China); Hu, Chenxian; Wang, Xiaofen; Wang, Hui; Liu, Xiuhui [Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province, College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China); Lu, Xiaoquan, E-mail: luxq@nwnu.edu.cn [Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province, College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070 (China)

    2017-02-28

    Highlights: • A sensitive non-enzymatic glucose sensor was explored by using a facile and green strategy. • Well dispersed and uniform NiHCF nanoparticles can be effectively produced by the introduction of electrochemical reduction graphene oxide films. • Metal hexacyanoferrate as a potential electron mediator was proposed and applied into non-enzymatic sensing. - Abstract: Rapid glucose detection is a key requirement for both diagnosis and treatment of diabetes. A facile and green strategy to achieve spherical-shaped nickel hexacyanoferrate (NiHCF) nanoparticals supported on electrochemical reduction graphene oxide by using electrochemical cyclic voltammetry is explored. As a sensing substrate, electrochemical reduction graphene oxide deposited on a glassy carbon electrode surface exhibited obvious positive effect on the electrodeposition of NiHCF nanoparticals with spherical structure and thus effectively improved the electrical conductivity and electrochemical sensing of the proposed amperometric sensor. Proof-concept experiments demonstrated that the proposed nanocomposites modified electrode exhibited excellent sensitivity toward glucose oxidation as well as with a satisfying detection limit of 0.11 μM. More importantly, we also explore that as a simple, green and facile method, electrochemical technology can be employed and provide a new strategy for developing GO and metal hexacyanoferrate based amperometric sensing platform toward glucose and other biomolecules.

  17. Sensitive endpoint detection for coulometric titration of microgram amounts of plutonium. Part II: Use of amperometric indication for the end point detection

    International Nuclear Information System (INIS)

    Chitnis, R.T.; Talnikar, S.G.; Thakur, V.A.

    1981-01-01

    Subsequent to the work on polarized indicator electrodes in the coulometric titration of PuO 2 2+ with electrolytically generated Fe 2+ , the possibility of applying amperometry for the endpoint detection in the same titration was explored. Earlier Moiseen et al used the amperometric indication in the coulometric titration of plutonium and have reported coefficient of variation of 0.4% for the titration of 1 mg of plutonium. The lowest amount of plutonium determined was in the range of 100 micrograms. In the present method, using similar analytical technique, the titrations of 25 micrograms and lower amounts of plutonium are reported. While titrating microgram amounts using amperometric indication, the residual currents due to the supporting electrolyte affect the titrations to a considerable extent. However, it is shown that by proper choice of the potential to be applied to the indicating electrode, the interference, due to the supporting electrolyte can be minimised. Using this technique, it is possible to titrate even a fraction of a microgram of plutonium. The precision at 0.5 microgram level is found to be about 6% and that for 5 micrograms, about 1%. (author)

  18. A green synthetic strategy of nickel hexacyanoferrate nanoparticals supported on the graphene substrate and its non-enzymatic amperometric sensing application

    International Nuclear Information System (INIS)

    Xue, Zhonghua; He, Nan; Rao, Honghong; Hu, Chenxian; Wang, Xiaofen; Wang, Hui; Liu, Xiuhui; Lu, Xiaoquan

    2017-01-01

    Highlights: • A sensitive non-enzymatic glucose sensor was explored by using a facile and green strategy. • Well dispersed and uniform NiHCF nanoparticles can be effectively produced by the introduction of electrochemical reduction graphene oxide films. • Metal hexacyanoferrate as a potential electron mediator was proposed and applied into non-enzymatic sensing. - Abstract: Rapid glucose detection is a key requirement for both diagnosis and treatment of diabetes. A facile and green strategy to achieve spherical-shaped nickel hexacyanoferrate (NiHCF) nanoparticals supported on electrochemical reduction graphene oxide by using electrochemical cyclic voltammetry is explored. As a sensing substrate, electrochemical reduction graphene oxide deposited on a glassy carbon electrode surface exhibited obvious positive effect on the electrodeposition of NiHCF nanoparticals with spherical structure and thus effectively improved the electrical conductivity and electrochemical sensing of the proposed amperometric sensor. Proof-concept experiments demonstrated that the proposed nanocomposites modified electrode exhibited excellent sensitivity toward glucose oxidation as well as with a satisfying detection limit of 0.11 μM. More importantly, we also explore that as a simple, green and facile method, electrochemical technology can be employed and provide a new strategy for developing GO and metal hexacyanoferrate based amperometric sensing platform toward glucose and other biomolecules.

  19. An amperometric penicillin biosensor with enhanced sensitivity based on co-immobilization of carbon nanotubes, hematein, and {beta}-lactamase on glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Chen Bi; Ma Ming [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081 (China); Su Xiaoli, E-mail: xsu@hunnu.edu.cn [Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research (Ministry of Education of China), College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081 (China)

    2010-07-26

    An amperometric penicillin biosensor with enhanced sensitivity was successfully developed by co-immobilization of multi-walled carbon nanotubes (MWCNTs), hematein, and {beta}-lactamase on glassy carbon electrode using a layer-by-layer assembly technique. Under catalysis of the immobilized enzyme, penicillin was hydrolyzed, decreasing the local pH. The pH change was monitored amperometrically with hematein as a pH-sensitive redox probe. MWCNTs were used as an electron transfer enhancer as well as an efficient immobilization matrix for the sensitivity enhancement. The effects of immobilization procedure, working potential, enzyme quantity, buffer concentration, and sample matrix were investigated. The biosensor offered a minimum detection limit of 50 nM (19 {mu}g L{sup -1}) for penicillin V, lower than those of the conventional pH change-based biosensors by more than two orders of magnitude. The electrode-to-electrode variation of the response sensitivity was 7.0% RSD.

  20. Polypyrrole-based bilayer nitrate amperometric biosensor with an integrated permselective poly-ortho-phenylenediamine layer for exclusion of inorganic interferences.

    Science.gov (United States)

    Adeloju, Samuel B; Sohail, Manzar

    2011-07-15

    A bilayer amperometric nitrate biosensor with an integrated permselective layer has been developed for exclusion of inorganic anion and cation interferences. The inner PPy(polypyrrole)-NaR-NADH layer of the biosensor is formed by galvanostatic polymerization of pyrrole (Py) in presence of nitrate reductase (NaR) and nicotinamide adenine dinucleotide (NADH), followed by formation of the outer permselective poly-ortho-phenylenediamine (P-o-PDA) layer by potentiodynamic polymerization of ortho-phenylenediamine (o-PDA). The exclusion efficiency (E(eff)) of the outer layer in rejecting inorganic cation and anion interferences is evaluated by a new proposed relationship. 73-87% and 47-84% of anion and cation interferences, respectively, were efficiently rejected with the permselective layer. Further improvement in the exclusion efficiency for cations was accomplished by combining the use of the outer layer with the addition of 1mM EDTA into the measurement solution. The addition of EDTA improved the E(eff) achieved for cation rejection by 10-40% to give net E(eff) of 89-94%. The inclusion of the outer layer also aided the retention of NaR and NADH in the inner PPy-NaR-NADH layer and, hence, enabled improved amperometric detection of nitrate, achieving a detection limit of 0.20 μM and a linear concentration range of 10-500 μM with a 3.4%rsd (n=10). Copyright © 2011 Elsevier B.V. All rights reserved.