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Injection Analysis (injection + analysis)
Kinds of Injection Analysis Selected AbstractsBarrel Plating Rhodium Electrode: Application to Flow Injection Analysis of HydrazineELECTROANALYSIS, Issue 14 2005Jun-Wei Sue Abstract We introduce here the application of barrel plating technology for mass production of disposable-type electrodes. Easy for mass production, barrel plating rhodium electrode (Rh-BPE) is for the first time demonstrated for analytical application. Hydrazine was chosen as a model analyte to elucidate the electrocatalytic and analytical ability of the Rh-BPE system in pH,7 phosphate buffer solution. Flow injection analysis (FIA) of hydrazine showed a linear calibration range of 25,1000,ppb with a slope and a regression coefficient of 5,nA/ppb and 0.9946, respectively. Twenty-two replicate injections of 25,ppb hydrazine showed a relative standard deviation of 3.17% indicating a detection limit (S/N=3) of 2.5,ppb. The system can be continuously operated for 1 day without any alteration in the FIA signals and is tolerable to the interference of oxalic acid, gelatine, Triton X-100, and albumin for even up to 100 times excess in concentration with respect to 400,ppb hydrazine. Since the fabrication cost of the electrode is cheap, it is thus disposable in nature. Furthermore, barrel plating technique can be extendable to other transition metals for application in many fields of research interest. [source] Flow Injection Analysis of Sulfide Using a Cinder/Tetracyano Nikelate Modified Screen-Printed ElectrodeELECTROANALYSIS, Issue 9 2005Jyh-Myng Zen Abstract Flow injection analysis (FIA) of sulfide is presented using a screen-printed carbon electrode modified with a cinder/tetracyano nickelate hybrid (designated as cinder/NiTcSPE). Hybridization of NiTc was achieved in iron-enriched industrial waste cinder material through the bimetallic formation of FeIII[NiII(CN)4]. The electrocatalytic oxidation of sulfide is mediated by the higher oxidation state of Ni in this hybrid-bimetallic complex. The system shows a detection limit (S/N=3) of 0.06,,M and a linear working range up to 1,mM in pH,10, 0.1,M KCl solution. Taking into account the relatively low volatility of the analyte in alkaline conditions, the system is ideally suited for the accurate detection of sulfide. The response of the electrode to sulfide is highly reproducible, thereby offering the potential development of a disposable amperometric sensor for sulfide. Selective detection of sulfide in cigarette smoke is presented in this study as an example of a real sample application. [source] Fast Mapping of Gunshot Residues by Batch Injection Analysis with Anodic Stripping Voltammetry of Lead at the Hanging Mercury Drop ElectrodeELECTROANALYSIS, Issue 2 2005Adriana De, Donato Abstract The forensic analysis of lead in gunshot residues (GSR) sampled on the hands of potential shooters is rendered faster, simpler and less expensive by a new batch injection analysis (BIA) method, based on differential pulse anodic stripping voltammetry (DPASV). A simple "J" shaped adaptor was designed to direct the flux of the analyte injected with a micropipettor onto the hanging mercury drop electrode of any commercial electrode stand. Sampling methods for GSR were compared and lifting with adhesive tape was elected for field use. The tapes are glued on polyethylene screens and stored in capped vials. Sampling with multiple strips provides coarse mapping of the distribution of lead on the shooter's hands. After a dissolution/extraction step with chloroform/aqueous 0.10,mol,L,1 HCl, 100,,L of the aqueous phase are injected during 25,s for accumulation of lead on the HMDE at ,0.60,V (vs. Ag/AgCl). A detection limit of 20,ng/mL of Pb(II), outreaching for GSR analysis, is reached without oxygen removal, at a frequency of 20 injections per hour. Results for sequences of shootings with a revolver and a pistol are presented. [source] Batch Injection Analysis: An Almost Unexplored Powerful ToolELECTROANALYSIS, Issue 7 2004Maria Abstract The main purpose of this review is to report the development and potentialities of batch injection analysis (BIA) and call the attention of researchers about the power of this (until now) almost unexplored tool. The text focuses on the concepts and potentialities of BIA combined with other techniques for analytical purposes. The association of BIA with amperometry, potentiometry, voltammetry, calorimetry, fluorescence and spectrophotometry is presented and important aspects related with each technique are discussed. Some aspects comparing the similarities and differences between BIA, FIA and wall-jet are presented along the text. [source] Determination of Epinephrine by Flow Injection Analysis Coupled Ag(III) Complex-Luminol Chemiluminescence DetectionCHINESE JOURNAL OF CHEMISTRY, Issue 4 2009Jiangbo BAI Abstract A new Ag(III) complex-luminol chemiluminescent system which was applied to the determination of epinephrine is firstly reported. Based on the enhancing effect of epinephrine on the chemiluminescence reaction of luminol with [Ag(HIO6)2]5, in alkaline solution, a highly sensitive chemiluminescence (CL) detection by flow injection analysis (FIA) was developed for epinephrine. Under the optimum conditions, CL intensity was proportional to concentration of epinephrine in the 1.0×10,9,1.0×10,7 mol·L,1 range. The limit of detection was 8.0×10,10 mol·L,1 for epinephrine (3,), with a relative standard deviation (n=11) of 2.9% for 1.5×10,8 mol·L,1 epinephrine. The method validation was done with epinephrine determinations in commercial pharmaceutical products. The mechanism of the reactions was also discussed. [source] A preliminary analysis and model of prostate injection distributionsTHE PROSTATE, Issue 4 2006Scott L. Chowning Abstract PURPOSE Understanding the internal dynamics of prostate injections, particularly injection pattern distribution is a key step to developing new therapies for prostate disease that may be best served with a direct injection approach. Due to excellent properties involving liquid contrast agents, MRI can be used for targeting and monitoring of injections into organs and tissues. MATERIALS AND METHODS Eleven intraprostatic injections were performed in vivo with canines using a custom transrectal guiding and imaging system for use in a standard 1.5 T MR scanner. In addition, 25 injections were performed on excised cadaveric human prostates, using a MedRad SpectrisÔ injector system. MRI was used to guide the injections and monitor intraparenchymal injection distribution. RESULTS T1 and T2-weighted MR images were correlated with histology to produce three-dimensional data sets that can be used to analyze trends in injection patterns. This analysis was used to develop strategies for injection prediction such as gadolinium preinjections and diffusion-weighted imaging guidance. In addition, a rough model of prostate injections is described, and a preliminary injection guide is developed that takes into account the individual clinician's goals for therapy. CONCLUSIONS MR visualization of injected therapeutic agents allows for prediction and monitoring of drug distributions, possibly improving efficacy and reducing side effects. Injection analysis and modeling may be used to assist in optimizing clinical treatments that require or would benefit from focal parenchymal injections into the prostate. © 2005 Wiley-Liss, Inc. [source] Fabrication of a Sensitive Cholesterol Biosensor Based on Cobalt-oxide Nanostructures Electrodeposited onto Glassy Carbon ElectrodeELECTROANALYSIS, Issue 24 2009Abdollah Salimi Abstract Electrodeposited cobalt oxide (CoOx) nanomaterials are not only used for immobilization of cholesterol oxidase (ChOx) but also as electron transfer mediator for oxidation of H2O2 generated in the enzymatic reaction. Voltammetry and flow injection analysis (FIA) were used for determination of cholesterol. FIA determination of cholesterol with biosensors yielded a calibration curve with the following characteristics: linear range up to 50,,M, sensitivity of 43.5,nA ,M,1 cm,2 and detection limit of 4.2,,M. The apparent Michaelis-Menten constant and the response time of the biosensor are 0.49,mM and 15,s, respectively. This biosensor also exhibits good stability, reproducibility and long life time. [source] Double Modification of Electrode Surface for the Selective Detection of Epinephrine and Its Application to Flow Injection Amperometric AnalysisELECTROANALYSIS, Issue 22 2009Guang-Ri Xu Abstract A glassy carbon electrode having two polymer layers has been applied to selectively detect epinephrine. The inner layer formed by electropolymerization of macrocyclic nickel complex functioned as an electrocatalyst for epinephrine oxidation and the outer layer composed of hydrolyzed polyurethane ,-benzyl L -glutamate as a screening layer. Differential pulse voltammetry showed almost 100% recovery of epinephrine even in 100-fold excess of interferents. When applied to a dual glassy carbon electrode as an amperometric detector in flow injection analysis, a linear response over 0.1,,M and 10,,M was obtained. Recovery tested for 5-fold diluted human urine samples was 97.5%. [source] Multiwalled Carbon Nanotubes Encased in Ruthenium Oxide Film as a Hybrid Material for Neurotransmitters SensorELECTROANALYSIS, Issue 16 2009Chien-Chieh Ti Abstract A hybrid film (MWCNTs-RuOx,nH2O) which contains multiwalled carbon nanotubes (MWCNTs) along with the incorporation of ruthenium oxide (RuOx,nH2O) has been synthesized on glassy carbon electrode (GCE), gold (Au), indium tin oxide (ITO) and screen printed carbon electrode (SPCE) by potentiostatic methods. The presence of MWCNTs in the hybrid film enhances surface coverage concentration (,) of RuOx,nH2O to ,2100%. The surface morphology of the hybrid film deposited on ITO has been studied using scanning electron microscopy and atomic force microscopy. These two techniques reveal that the RuOx,nH2O incorporated on MWCNTs. Electrochemical quartz crystal microbalance study too reveals the incorporation of MWCNTs and RuOx,nH2O. The MWCNTs-RuOx,nH2O hybrid film exhibits promising enhanced electrocatalytic activity towards the biochemical compounds such as epinephrine and norepinephrine. The electrocatalytic responses of these analytes at RuOx,nH2O, MWCNTs and MWCNTs-RuOx,nH2O hybrid films have been measured using cyclic voltammetry. The obtained sensitivity values from electrocatalysis studies of analytes for MWCNTs-RuOx,nH2O hybrid film are higher than the RuOx,nH2O and MWCNTs films. Finally, the flow injection analysis has been used for the amperometric studies of analytes at MWCNTs-RuOx,nH2O hybrid film modified SPCEs. [source] Integrating an Enzyme-Entrapped Conducting Polymer Electrode and a Prereactor in a Microfluidic System for Sensing GlucoseELECTROANALYSIS, Issue 6 2008Po-Chin Nien Abstract In this study, the flow injection analysis was applied to the enzyme-entrapped electrode on a chip for sensing glucose. The on-chip microelectrode was fabricated by the standard photolithography in clean-room environment and the microfluidic channel height of 100,,m on the chip was formed by poly(dimethylsiloxane). The conducting polymer, poly(3,4-ethylenedioxythiophene), PEDOT, was electropolymerized to entrap the coexisting glucose oxidase (GOD) by cyclic voltammetry (CV). The amount of enzyme entrapped in the matrix measured spectroscopically was about 0.101,U/cm2. At a flow rate of 10,ml/hr, the working electrode (Pt/PEDOT/GOD, WE1) was set at 0.7,V (vs. Ag/AgCl) and sensing of H2O2 was carried out by injecting samples with various concentrations of glucose (Glu). A linear relationship between the sensing current and the glucose concentration, ranging from 1 to 20,mM, was obtained with a sensitivity of 8,nA mm,2 mM,1. The response time and the recovery time were about 30 and 230,s, respectively. For a single-potential test, the oxidation currents of 0.08,mM ascorbic acid (AA) and a blend of 0.08,mM AA and 10,mM Glu reached 31.3% and 145.5%, respectively, when compared with the oxidation current of 10,mM Glu alone. However, when a pre-reactor (WE2) was set at the same potential (0.7,V) before the main enzyme integrated electrode (WE1), the oxidation current for the above mixed solution reached 99.6% of the original one. [source] Direct Electrochemical Sensing and Detection of Natural Antioxidants and Antioxidant Capacity in Vitro SystemsELECTROANALYSIS, Issue 22 2007Antonio, Javier Blasco Abstract This review highlights the role of electrochemical approaches in the sensing of antioxidants and their antioxidant capacity with especial attention to the analytical possibilities of electrochemistry in the direct evaluation of antioxidant capacity exhibited by food and biological samples due to the termed dietary, natural or biological antioxidants (mainly polyphenols, and vitamins C and E). The analytical potency of the electrochemistry is comprehensively stated and the selected results found in the literature are summarized and discussed critically. The main electrochemical approaches used have been cyclic voltammetry (CV) and flow injection analysis with amperometric detection (FIA-ED). In addition, miniaturization is going to break new frontiers in the evaluation of antioxidant activity. [source] Zinc Oxide/Zinc Hexacyanoferrate Hybrid Film-Modified Electrodes for Guanine DetectionELECTROANALYSIS, Issue 18 2007Hung-Wei Chu Abstract An electroactive polynuclear hybrid films of zinc oxide and zinc hexacyanoferrate (ZnO/ZnHCF) have been deposited on electrode surfaces from H2SO4 solution containing Zn(NO3)2 and K3[Fe(CN)6] by repetitive potential cycling method. Simultaneous cyclic voltammetry and electrochemical quartz crystal microbalance (EQCM) measurements demonstrate the steady growth of hybrid film. There are two redox couples present in the voltammograms of hybrid film and it is obvious in the case of pH,2. Surface morphology of hybrid film was investigated using scanning electron microscopy (SEM) and atomic force microscopy (AFM). Energy dispersive spectrometer (EDS) data confirm existence of zinc oxide in the hybrid film. The effect of type of monovalent cations on the redox behavior of resulting film was investigated. In pure supporting electrolyte, electrochemical responses of modified electrode resemble with that of a surface immobilized redox couple. The electrocatalytic activity of ZnO/ZnHCF hybrid film was investigated towards guanine using cyclic voltammetry and rotating disc electrode (RDE) techniques. Finally, feasibility of using ZnO/ZnHCF hybrid film-coated electrodes for guanine estimation in flow injection analysis (FIA) was also investigated. [source] Electrochemical Preparation of Poly(Malachite Green) Film Modified Nafion-Coated Glassy Carbon Electrode and Its Electrocatalytic Behavior Towards NADH, Dopamine and Ascorbic AcidELECTROANALYSIS, Issue 14 2007Shen-Ming Chen Abstract Poly(malachite green) film modified Nafion-coated glassy carbon electrodes have been prepared by potentiodynamic cycling in malachite green solution. The pH of polymerisation solution has only minor effect on film formation. Electrochemical quartz crystal microbalance (EQCM) was used to monitor the growth of the poly(malachite green) film. Cyclic voltammogram of the poly(malachite green) film shows a redox couple with well-defined peaks. The redox response of the modified electrode was found to be depending on the pH of the contacting solution. The peak potentials were shifted to a less positive region with increasing pH and the dependence of the peak potential was found to be 56,mV per pH unit. The electrocatalytic behavior of poly(malachite green) film modified Nafion-coated glassy carbon electrodes was tested towards oxidation of NADH, dopamine, and ascorbic acid. The oxidation of dopamine and ascorbic acid occurred at less positive potential on poly(malachite green) film compared to bare glassy carbon electrode. In the case of NADH, the overpotential was reduced substantially on modified electrode. Finally, the feasibility of utilizing poly(malachite green) film electrode in analytical estimation of ascorbic acid was demonstrated in flow injection analysis. [source] Electroanalytical Approach to Evaluate Antioxidant Capacity in Honeys: Proposal of an Antioxidant IndexELECTROANALYSIS, Issue 18 2006Mónica Ávila Abstract A novel electrochemical route to estimate the antioxidant capacity in honey samples is proposed just using flow injection analysis. The analytical strategy involved the selective oxidation of polyphenolic compounds using two different target potentials, +0.8 and +0.5,V, at two different pHs. An oxidation current obtained at the fixed potential was used as an analytical guide of the antioxidant activity of the target honeys. Chemometrics (correlation and principal component analysis, PCA) demonstrated the significance of the electrochemical protocol versus the traditional spectrophotometric ones in the evaluation of antioxidant capacity and revealed the role of detection potential as a screening variable. The proposed protocol is very simple and fast. However, the most relevant merit of the electrochemical procedure is its inherent versatility which allows the evaluation of the antioxidant activity under predesigned controlled oxidation conditions. In addition, since intercept was statistically zero, its corresponding antioxidant content using just a calibration factor is proposed thus simplifying the calibration-analysis process. As a result, an electrochemical antioxidant index (EAI) is proposed. [source] FIA Determination of Paracetamol in Pharmaceutical Drugs by Using Gold Electrodes Modified with a 3-Mercaptopropionic Acid MonolayerELECTROANALYSIS, Issue 9 2006Valber Abstract A flow injection analysis (FIA) method for the determination of paracetamol in pharmaceutical drugs using a gold electrode modified with a self-assembled monolayer (SAM) of 3-mercaptopropionic acid is described. At optimized experimental conditions the dynamic concentration range was 0.15 to 15.0,mg L,1 with a detection limit of 0.2,,g mL,1 (S/N=3). The repeatability of current responses for injections of 10,,mol L,1 paracetamol was evaluated to be 3.2% (n=30) and the analytical frequency was 180,h,1. The lifetime of the modified electrode was found to be 15 days. The results obtained by using the proposed amperometric method for paracetamol determination in four different drug samples compared well with those found by spectrophotometry. [source] A LiMn2O4 Based Electrochemical Scheme for Selective Measurement of DopamineELECTROANALYSIS, Issue 3 2006Hoang, Jyh Leu Abstract A new cathodic scheme was developed for the determination of dopamine by flow injection analysis (FIA). A mild oxidizing agent, lithium manganese (III, IV) oxide (LiMn2O4), as an upstream modifier can oxidize the dopamine to produce the dopaminequinone, and then the oxidized product is subsequently detected by the downstream detector at ,0.1,V (vs. Ag/AgCl). In this work, the significant feature of LiMn2O4 based sensing scheme possesses no interference from other tested biological amines including acetylcholine, epinephrine, glutamate, and histamine. Otherwise, there is no detectable interference from ascorbic acid, but 2% and 1% negligible interferences were found from uric acid and acetaminophen, respectively. [source] Barrel Plating Rhodium Electrode: Application to Flow Injection Analysis of HydrazineELECTROANALYSIS, Issue 14 2005Jun-Wei Sue Abstract We introduce here the application of barrel plating technology for mass production of disposable-type electrodes. Easy for mass production, barrel plating rhodium electrode (Rh-BPE) is for the first time demonstrated for analytical application. Hydrazine was chosen as a model analyte to elucidate the electrocatalytic and analytical ability of the Rh-BPE system in pH,7 phosphate buffer solution. Flow injection analysis (FIA) of hydrazine showed a linear calibration range of 25,1000,ppb with a slope and a regression coefficient of 5,nA/ppb and 0.9946, respectively. Twenty-two replicate injections of 25,ppb hydrazine showed a relative standard deviation of 3.17% indicating a detection limit (S/N=3) of 2.5,ppb. The system can be continuously operated for 1 day without any alteration in the FIA signals and is tolerable to the interference of oxalic acid, gelatine, Triton X-100, and albumin for even up to 100 times excess in concentration with respect to 400,ppb hydrazine. Since the fabrication cost of the electrode is cheap, it is thus disposable in nature. Furthermore, barrel plating technique can be extendable to other transition metals for application in many fields of research interest. [source] Flow Injection Analysis of Sulfide Using a Cinder/Tetracyano Nikelate Modified Screen-Printed ElectrodeELECTROANALYSIS, Issue 9 2005Jyh-Myng Zen Abstract Flow injection analysis (FIA) of sulfide is presented using a screen-printed carbon electrode modified with a cinder/tetracyano nickelate hybrid (designated as cinder/NiTcSPE). Hybridization of NiTc was achieved in iron-enriched industrial waste cinder material through the bimetallic formation of FeIII[NiII(CN)4]. The electrocatalytic oxidation of sulfide is mediated by the higher oxidation state of Ni in this hybrid-bimetallic complex. The system shows a detection limit (S/N=3) of 0.06,,M and a linear working range up to 1,mM in pH,10, 0.1,M KCl solution. Taking into account the relatively low volatility of the analyte in alkaline conditions, the system is ideally suited for the accurate detection of sulfide. The response of the electrode to sulfide is highly reproducible, thereby offering the potential development of a disposable amperometric sensor for sulfide. Selective detection of sulfide in cigarette smoke is presented in this study as an example of a real sample application. [source] Fast Mapping of Gunshot Residues by Batch Injection Analysis with Anodic Stripping Voltammetry of Lead at the Hanging Mercury Drop ElectrodeELECTROANALYSIS, Issue 2 2005Adriana De, Donato Abstract The forensic analysis of lead in gunshot residues (GSR) sampled on the hands of potential shooters is rendered faster, simpler and less expensive by a new batch injection analysis (BIA) method, based on differential pulse anodic stripping voltammetry (DPASV). A simple "J" shaped adaptor was designed to direct the flux of the analyte injected with a micropipettor onto the hanging mercury drop electrode of any commercial electrode stand. Sampling methods for GSR were compared and lifting with adhesive tape was elected for field use. The tapes are glued on polyethylene screens and stored in capped vials. Sampling with multiple strips provides coarse mapping of the distribution of lead on the shooter's hands. After a dissolution/extraction step with chloroform/aqueous 0.10,mol,L,1 HCl, 100,,L of the aqueous phase are injected during 25,s for accumulation of lead on the HMDE at ,0.60,V (vs. Ag/AgCl). A detection limit of 20,ng/mL of Pb(II), outreaching for GSR analysis, is reached without oxygen removal, at a frequency of 20 injections per hour. Results for sequences of shootings with a revolver and a pistol are presented. [source] Characterization and Assessment of the Microjet Electrode as a Detector for HPLCELECTROANALYSIS, Issue 9 2004Susan Cannan Abstract The microjet electrode (MJE) is characterized as a detector for high performance liquid chromatography (HPLC). Voltammetric measurements of the oxidation of hydroquinone (HQ) allow mass transport to be determined for the MJE detector configuration, and the factors controlling the conversion efficiency of the device to be well understood. The current-time response to the flow injection analysis of volumes of solution in the 10,80,,L range has been established, and the limit of detection of this method has been determined. The latter was found to approach that of UV absorbance measurements, which is particularly encouraging, given that HQ has a relatively strong chromophore (,=2,290.8,cm,1 mol,1,L). This detection system is a robust and simple arrangement with the capability of analyzing large volumes of eluent at typical analytical HPLC flow rates. [source] Batch Injection Analysis: An Almost Unexplored Powerful ToolELECTROANALYSIS, Issue 7 2004Maria Abstract The main purpose of this review is to report the development and potentialities of batch injection analysis (BIA) and call the attention of researchers about the power of this (until now) almost unexplored tool. The text focuses on the concepts and potentialities of BIA combined with other techniques for analytical purposes. The association of BIA with amperometry, potentiometry, voltammetry, calorimetry, fluorescence and spectrophotometry is presented and important aspects related with each technique are discussed. Some aspects comparing the similarities and differences between BIA, FIA and wall-jet are presented along the text. [source] Nanoparticle-Structured Ligand Framework as Electrode InterfacesELECTROANALYSIS, Issue 1-2 2004Nancy Abstract Nanostructured thin film assemblies derived from metal or oxide nanocrystal cores and functionalized molecular shells provide large surface-to-volume ratio and three-dimensional ligand frameworks. In this article, we report results of an investigation of the nanostructured materials for electroanalysis. Monolayer-capped gold nanoparticles of 2-nm core diameter and carboxylic acid-functionalized alkyl thiols were assembled on electrode surfaces via an exchange-crosslinking-precipitation reaction route, and were studied as a model system. The network assemblies exhibit open frameworks in which the void space forms channels with the nanometer sized cores defining its size and the shell structures defining its chemical specificity. Such nanostructures were exploited to demonstrate the viability of responsive materials for interfacial incorporation and fluxes of ionic species. The nanomaterials were characterized by an array of techniques, including cyclic voltammetry, electrochemical quartz-crystal nanobalance, flow injection analysis, and surface infrared reflection spectroscopy. The current responses and mass loading as a result of the incorporation of ionic species into the nanostructure have been analyzed. The potential application of the nanostructured thin films for electrochemical detection in microfluidic systems is also discussed. [source] New Strategy for Dehydrogenase Amperometric Biosensors Using Surfactant to Enhance the Sensitivity of Diaphorase/Ferrocene Modified Carbon Paste Electrodes for Electrocatalytic Oxidation of NADHELECTROANALYSIS, Issue 13 2003César Ramírez-Molina Abstract A carbon paste electrode (CPE) modified with diaphorase (DAP) and ferrocene (FcH) has been developed for determination of NADH at low working potential. The sensitivity and operational stability, towards the detection of the reduced form of the nicotinamide adenine dinucleotide (NADH) in flow injection analysis (FIA), were greatly improved (5 times) upon adding Tween 20 into the electrode matrix. The magnitude of the amperometric signal was dependent on DAP, FcH and surfactant loading, into the modified carbon paste electrode. A rapid and repeatable response was observed to the variation of NADH concentration in the vicinity of the electrode surface. Such advantages of the DAP/FcH/Tween 20 modified carbon paste were successfully used in the construction of L -lactate dehydrogenase modified electrodes. The use of this new approach can be generalized to other dehydrogenases and represents a decisive step for a versatile preparation method of amperometric biosensors. [source] Carbon nanotube/poly(methyl methacrylate) composite electrode for capillary electrophoretic measurement of honokiol and magnolol in Cortex Magnoliae OfficinalisELECTROPHORESIS, Issue 16 2006Xiao Yao Abstract This paper describes the development and the application of a novel carbon nanotube/poly(methyl methacrylate) (CNT/PMMA) composite electrode as a sensitive amperometric detector of CE. The composite electrode was fabricated on the basis of the in,situ polymerization of a mixture of CNT and prepolymerized methylmethacrylate in the microchannel of a piece of fused-silica capillary under heat. The performance of this unique system has been demonstrated by separating and detecting honokiol and magnolol in traditional Chinese medicine, Cortex Magnoliae Officinalis. Factors influencing their separation and detection processes were examined and optimized. Honokiol and magnolol were well separated within 7,min in a 40 cm long capillary at a separation voltage of 15,kV using a 50 mM borate buffer (pH,9.2). The new CNT-based CE detector offered significantly lower operating potentials, yielded substantially enhanced S/N characteristics, and exhibited resistance to surface fouling and hence enhanced stability. It demonstrated long-term stability and reproducibility with RSDs of less than 5% for the peak current (n = 9) and should also find a wide range of applications in microchip CE, flowing injection analysis, and other microfluidic analysis systems. [source] Identification and quantification of in vitro adduct formation between protein reactive xenobiotics and a lysine-containing model peptideENVIRONMENTAL TOXICOLOGY, Issue 1 2003Peter Reichardt Abstract Formation of in vitro adducts between different classes of xenobiotics and the lysine-containing peptide Lys-Tyr was monitored by high-performance liquid chromatography and electrospray ionization mass spectrometry. The molecular structures of the main resulting products could be sensitively analyzed by mass spectrometry (flow injection analysis), enabling the detection of characteristic binding formations. Aldehydes such as formaldehyde, acetaldehyde, and benzaldehyde were shown to form stable linkages to lysine amino groups via Schiff bases. Other electrophilic substances (e.g., toluene-2,4-diisocyanate, 2,4-dinitro-1-fluorobenzene, 2,4,6-trinitrobenzene sulfonic acid, dansyl chloride, and phthalic acid anhydride) also formed covalent adducts with lysine residues. The reactivity of the compounds was quantified by measuring the amount of peptide that remained unchanged after incubation for a certain period with the xenobiotic. Although reactivity levels within this group of aldehydes varied only to a small extent, as would be expected, extreme differences were seen among the structurally heterogeneous group of nonaldehyde xenobiotics. These results support the hypothesis that simple chemical reactions may lead to the adduction of nucleophilic macromolecules such as peptides or proteins. Such reactions, in particular, Schiff base formation of aldehydes, have previously been shown to be capable of specifically interfering with costimulatory signaling on T cells. Our results suggest that electrophilic xenobiotics of other classes may also inherit the capacity to exert similar effects. Forming covalent linkage to peptides may represent a possible molecular mechanism of electrophilic xenobiotics in vivo, yielding immunotoxic effects. The model utilized in this study is appropriate for monitoring the adduction of xenobiotics to basic peptides and for analyzing the resulting molecular structures. © 2003 Wiley Periodicals, Inc. Environ Toxicol 18: 29,36, 2003. [source] Determination of propafenone hydrochloride by flow-injection analysis coupled with resonance light scattering detectionLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 2 2009Xiaoli Hu Abstract A simple, sensitive and rapid flow injection analysis (FIA) method with resonance light scattering (RLS) was described for the determination of propafenone (PPF). The method was based on the ion-association reaction of 12-tungstophosphoric acid (TP) with propafenone. In pH 1.0 acidic medium, TP reacted with PPF to form an ion-associate complex, which resulted in a significant enhancement of RLS intensity. The maximum scattering peak was located at 340 nm, the RLS intensity was proportional to the concentration of PPF in the range 0.003,9.0 µg/mL, and the detection limit (3,) of 1.0 ng/mL was obtained at a sampling rate of 60 samples/h. The feasible reaction conditions and FIA parameters for the system were optimized. The method proposed in this paper shows satisfactory reproducibility with a relative standard deviation (RSD) of 2.1% for 10 successive determinations of 2.0 µg/mL PPF. The present method had been successfully applied to the determination of PPF in serum samples and pharmaceutical samples. The results obtained were in agreement with the method used in the Chinese Pharmacopoeia. Copyright © 2008 John Wiley & Sons, Ltd. [source] Chemiluminescence determination of chlorpheniramine using tris(1,10-phenanthroline),ruthenium(II) peroxydisulphate system and sequential injection analysisLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 1 2009Fakhr Eldin O. Suliman Abstract A sequential injection (SI) method was developed for the determination of chlorpheniramine (CPA), based on the reaction of this drug with tris(1,10-phenanthroline),ruthenium(II) [Ru(phen)32+] and peroxydisulphate (S2O82,) in the presence of light. The instrumental set-up utilized a syringe pump and a multiposition valve to aspirate the reagents [Ru(phen)32+ and S2O82,] and a peristaltic pump to propel the sample. The experimental conditions affecting the chemiluminescence reaction were systematically optimized, using the univariate approach. Under the optimum conditions linear calibration curves of 0.1,10 µg/ml were obtained. The detection limit was 0.04 µg/ml and the relative standard deviation (RSD) was always < 5%. The procedure was applied to the analysis of CPA in pharmaceutical products and was found to be free from interferences from concomitants usually present in these preparations. Copyright © 2008 John Wiley & Sons, Ltd. [source] Flow injection analysis of tetracyclines using inhibited Ru(bpy)32+/tripropylamine electrochemiluminescence systemLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 1 2005Yong-Qiang Pang Abstract Tetracyclines (TCs) were found to strongly inhibit the electrochemiluminescence (ECL) from the Ru(bpy)32+,tripropylamine system when a working Pt electrode was maintained at 1.05 V (vs. Ag[sol ]AgCl) in pH 8.0 carbonate buffer solution. On this basis, a flow injection (FI) procedure with inhibited electrochemiluminescence detection has been developed for the determination of tetracycline (TC) and oxytetracycline (OTC). Under the optimized condition, the linear ranges of 2.0 × 10,8,1.0 × 10,5 and 1.0 × 10,8,1.0 × 10,5 g[sol ]mL and the detection limits of 4.0 × 10,9 and 3.8 × 10,9 g[sol ]mL were obtained for TC and OTC, respectively. The relative standard deviations (RSD) were 0.68% and 1.18% for 5.0 × 10,7 g[sol ]mL TC and OTC (n = 13), respectively. The method showed higher sensitivity than most of the reported methods. It was successfully applied to the determination of tetracycline in a Chinese proprietary medicine, Tetracyclini and Cortisone Eye Ointment, and the residues of tetracycline in honey products. The inhibition mechanism has been proposed due to an energy transfer between electrogenerated Ru(bpy)32+* and benzoquinone derivatives at the electrode surface. Copyright © 2005 John Wiley & Sons, Ltd. [source] Electrogenerated chemiluminescence of luminol for oxidase-based fibre-optic biosensorsLUMINESCENCE: THE JOURNAL OF BIOLOGICAL AND CHEMICAL LUMINESCENCE, Issue 2 2001Christophe A. Marquette Abstract The luminol electrochemiluminescence has been exploited for the development of several fibre-optic biosensors allowing the detection of hydrogen peroxide and of substrates of H2O2 -producing oxidases. Electro-optical flow injection analysis of glucose, lactate, cholesterol and choline are thus described. To perform the experiments, a glassy carbon electrode was polarized at a fixed potential. Luminol was then electrochemically oxidized and could react in the presence of hydrogen peroxide to produce light. Several parameters had to be optimized to obtain reliable optical biosensors. An optimum applied potential of +425 mV between the glassy carbon electrode and the platinum pseudo-reference electrode was determined, allowing the best signal: noise ratio to be obtained. It was also necessary to optimize the experimental conditions for the immobilization of the different oxidases involved (preactivated membranes, chemically activated collagen membranes, photopolymerized matrix). For each biosensor developed, the optimum reaction conditions have been studied: buffer composition, pH, temperature, flow rate and luminol concentration. Under optimal conditions, the detection limits (S/N,=,3) were 30,pmol, 60,pmol, 0.6,nmol and 10,pmol for lactate, glucose, cholesterol and choline, respectively. The miniaturization of electrochemiluminescence-based biosensors has been realized using screen-printed electrodes instead of a glassy carbon macroelectrode, with choline oxidase as a model H2O2 -generating oxidase. Copyright © 2001 John Wiley & Sons, Ltd. [source] Determination of lead content in medicinal plants by pre-concentration flow injection analysis,flame atomic absorption spectrometryPHYTOCHEMICAL ANALYSIS, Issue 6 2009Marina M. A. Campos Abstract Introduction , Although medicinal plants are widely used throughout the world, few studies have been carried out concerning the levels of heavy metal contaminants present. Such metals are highly toxic to living organisms even in low concentrations owing to their cumulative effect. The present paper describes the the development of a pre-concentration flow injection analysis-flame atomic absorption spectrometric system to determine the lead content in medicinal plants at the ppb level. Objective , To develop a pre-concentration flow injection analysis-flame atomic absorption spectrometric system to determine the lead content in medicinal plants at the ppb level. Methodology , A pre-concentration flow system was coupled to a flame atomic absorption spectrometer. The plant samples were analysed after nitroperchloric digestion. The proposed system was optimised by evaluating the following parameters: nature, concentration and volume of the eluent solution, elution flow rate, elution efficiency, pre-concentration flow rate and pre-concentration time. Results , The proposed system exhibited good performance with high precision and repeatability (RSD , 2.36%), excellent linearity (r = 0.9999), low sample consumption (10.5 mL per determination) and an analytical throughput of 55 samples/h. Lead concentrations ranged from 3.37 ± 0.25 to 7.03 ± 0.51 ,g/g in dry material. This concentration interval is greater than that previously published in the literature. Conclusion , The inclusion of a pre-concentration column in the flow manifold improved the sensitivity of the spectrometer. Thus, it was possible to determine the analyte at the ng/mL level in sample solutions of medicinal plants. This is a very important accomplishment, especially when the cumulative effect of heavy metals in living organisms is considered. Copyright © 2009 John Wiley & Sons, Ltd. [source] | ||||||||||||||||