Application of Adsorptive Stripping Voltammetry for the Nano‐Level Detection of Tramadol in Biological Fluids and Tablets Using Fast Fourier Transform Continuous Cyclic Voltammetry at an Au Microelectrode in a Flowing System

Abstract

A novel adsorptive fast Fourier transform cyclic voltammetry (AFFTCV) technique for the fast determination of tramadol in flow‐injection systems has been introduced in this work. The potential waveform, consisting of the potential steps for cleaning, stripping, and potential ramp, was continuously applied on an Au disk microelectrode (with a 12.5 µm in radius). The proposed detection method has some advantages, the greatest of which are as follows: first, it is no more necessary to remove oxygen from the analyte solution and second, it is a very fast and appropriate technique for determination of the drug compound in a wide variety of chromatographic analysis methods. The influences of pH of eluent, accumulation potential, sweep rate, and accumulation time on the determination of the tramadol were considered. The method was linear over the concentration range of 1.5–900,000 pg/ml (r=0.9968) with a limit of detection and quantitation 0.32 and 1.5 pg/ml, respectively. The method has the requisite accuracy, sensitivity, precision, and selectivity to assay tramadol in tablets and in biological fluids.     

Tartaric Acid Modified Electrodes and Studies on its Application for the Anodic striphing Voltammetry of cu(Ⅱ)

The preparation of tartaric acid modified electrode was studied.Reaction mechanism of copper(Ⅱ) on tartaric acid modified electrode was discussed and determination conditions for trace Cu(Ⅱ) by ASV were also founded.     

Application of the Bismuth Film Electrode for Catalytic Adsorptive Stripping Potentiometric Determination of Cobalt in Dimethylglyoxime‐Nitrite System

Abstract

The application of bismuth film electrodes to the determination of cobalt by constant current adsorptive stripping potentiometry with exploitation of a catalytic effect is presented. The addition of NaNO₂ to the solution containing ammonia buffer and dimethylglyoxime results in a 25‐fold enhancement of the adsorptive stripping potentiometric cobalt signal. Several key parameters of the potentiometric stripping mode were optimized, including the composition of the supporting electrolyte, the stripping current, the accumulation potential, and the accumulation time. The optimized procedure yields favorable and highly stable stripping responses with good precision (RSD=1.4% for a Co concentration of 2 µg L^?1), low detection limit (0.07 µg L^?1), and good linearity (up to 10 µg L^?1, R²=0.998) with a deposition time of 60 s and a stripping current of 10 µA. The method enables the determination of Co in the presence of high excesses of Ni or Zn.     

Determination of Chlorfenvinphos in Soils by Microwave‐Assisted Extraction and Stripping Voltammetry with an Ultramicroelectrode

Abstract

A methodology for the determination of the pesticide chlorfenvinphos by microwave‐assisted solvent extraction and square‐wave cathodic stripping voltammetry at a mercury film ultramicroelectrode in soil samples is proposed. Optimization of microwave solvent extraction performed with two soils, selected for having significantly different properties, indicated that the optimum solvent for extracting chlorfenvinphos is hexane‐acetone (1∶1, v/v). The voltammetric procedure is based on controlled adsorptive accumulation of the insecticide at the potential of?0.60 V (vs. Ag/AgCl) in the presence of Britton‐Robinson buffer (pH 6.2). The detection limit obtained for a 10 s collection time was 3.0×10^?8 mol l^?1. The validity of the developed methodology was assessed by recovery experiments at the 0.100 µg g^?1 level. The average recoveries and standard deviations for the global procedure reached by MASE‐square‐wave voltammetry were 90.2±2.8% and 92.1±3.4% for type I (soil rich in organic matter) and type II (sandy soil) samples, respectively. These results are in accordance to the expected values which show that the method has a good accuracy.     

Aqueous Long-Term Solubility of Titania Nanoparticles and Titanium(IV) Hydrolysis in a Sodium Chloride System Studied by Adsorptive Stripping Voltammetry

The solubility of industrially produced titanium dioxide nanoparticles has been studied in aqueous sodium chloride media in the pH range 1 to 13 at 25 °C by using adsorptive stripping voltammetry (AdSV). Kinetic dissolution curves have been obtained as well as long-term solubilities that provide an approximation of the equilibrium solubilities. The titania nanoparticles used in the dissolution experiments have been characterized by nitrogen sorption measurements, XRD and colloid titration. The equilibrium solubilities and titanium(IV) speciation and their dependences on pH have been modelled by assuming the formation of the mononuclear titanium hydroxo complexes [Ti(OH) _n ]⁽⁴⁻ⁿ⁾⁺ (n=2 to 5) to be the only titanium species present. The solubility product of titanium dioxide and equilibrium constants for titanium(IV) hydrolysis, calculated from the AdSV solubility data, are presented.     

Catalytic Adsorptive Stripping Voltammetry at a Carbon Paste Electrode for the Determination of Amiodarone

Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and overelaborate operation procedures. The use of the chemical catalysis of oxidant on the reduction product of analyte not only can eliminate the contamination of analyte to solid electrodes but also can improve the faradaic response of analyte. This work introduced both the catalysis of oxidant K2S2O8 and the enhancement of surfactant Triton X-100 on the faraday response of amiodarone into an adsorptive stripping voltammetry at a carbon paste electrode for the determination of amiodarone. The method exhibits high sensitivity, good reproducibility and simple operation procedure. In 0.2 mol·L^-1 HOAc-NaOAc buffer （pH=5.3） containing 2.2×10^-2 mol·L^-1 K2S2O8 and 0.002% Triton X-100, the 2.5th-order derivative stripping peak current of the catalytic wave at 0.3 V （vs. Ag/AgCl） is rectilinear to amiodarone concentration in the range of 2.0×10^-10-2.3×10^-8 mol·L^-1 with a detection limit of 1.5×10^-10 mol·L^-1 after accumulation at 0 V for 30 s.     

Assessment of the Stability of a Mercury Film on a Glass–Ceramic Carbon Electrode when Determining Zinc in the Presence of Manganese by Anodic Stripping Voltammetry

The possibility of assessing the stability of operation of a mercury film graphite electrode in anodic stripping voltammetry using Shewhart control charts (CCs) is shown. The offered technique allows significantly increasing the efficiency of the voltammetric determination of zinc and manganese and taking measurements of analytes in samples during a working day without replacing the mercury film on the electrode surface.     

Nature of a Positive Anodic Peak in the Stripping Voltammogram of Binary Platinum–Metal Systems

The effect of platinum on the electrodeposition of cadmium, lead, copper, and mercury at the surface of a solid electrode was studied by stripping voltammetry. It was shown that an additional current peak in the anodic voltammogram corresponded to the metal ionization to support electrolytic platinum.     

Secondary Activation of Commercial Activated Carbon and its Application in Electric Double Layer Capacitor

The cheap commercial activated carbon (AC) was improved through the secondary activation under steam in the presence of FeCl2 catalyst in the temperature range of 800-950℃ and its application in electric double layer capacitors(EDLCs) with organic electrolyte was studied. The re-acivation of AC results in the increases in both specific capacitance and high rate capability of DELCs. For AC treated under optimized conditions, its discharge specific capacitance increases up to 55.65F/g, an increase of about 33% as compared to the original AC, and the high rate capability was increased significantly.The good performances of EDLC with improved AC were correlated to the increasing mesoporous ratio.     

Study of RLT Filtration for Staircase and Normal Pulse Voltammetry

INTRODUCTIoNFuChinSoongandJ.T.MaloY'lproposedanewway,whichwascalledRLT(Riemann-Liouvilletransform)POlarography,toseparaefaradaiccurrentfromcapacitivecurrentinpolarography.Then,M.R.HemsteadandK.B.Oldhaml2lproposedCottrelfiltraion.TheprincipleofthesetWomethodswasbasedontheimportantproPertyoffractionalintegrationanddifferentiation:Accordingtothisprinciple,weproposedRLTfiltrationwhichcouldbeappliedintwokindsofpotentialstepscanvoltammetry--Staircaseandnormalpulsevoltammetry.THEoRYT…     

Use of Differential Pulse Polarography and Adsorptive Stripping Tensammetry for Investigation of Gas Stripping Separation Of Nonionic Surfactants

Methods for determination of nonionic surfactants in surface water and wastewater have not been satisfactory since yet. Wickbold's method is commonly used forsuch a purpose (1). This method consists of three time-consuming stages: (i) gas stri-pping separation of nonionic surfactants from water matrix, (ii) precipitation of ethox-     

Resonance Light Scattering Spectra of Silver Thiocyanate System and its Application in Analysis

A novel determination method of Ag^＋ was established. In acetic acid-sodium acetate buffer （pH 5.0） medium, Ag^＋ reacts with SCN^- to form AgSCN in the presence of TritonX-100,which results in an increase of resonance light scattering （RLS）and giving a new RLS spectrum.The maximum RLS peak was at 585 nm,The enhancement of resonance light scattering at 585 nm was proportional to the concentration of Ag^＋ ranging from 0.0045-4.00μg mL^-1 （r=9991）,and the detection limit was 1.37 ng mL^-1 with the recovery of 97.70%- 104.80%。     

Adsorptive Stripping Voltammetry of 9‐Phenanthrol in the Presence of Copper at the Static Mercury Drop Electrode—Basis for Quantitative Determination of PAH Metabolite in Biological Materials

Abstract

The electrochemical behavior of 9‐phenanthrol in the presence of copper (II) at a static mercury drop electrode was investigated to provide the basis for development of an inexpensive, sensitive, and reliable method for determination of polycyclic aromatic hydrocarbon (PAH) metabolites in biological matrices. Optimum experimental conditions for analytical applications were obtained in 0.005 M NaOH solution using an accumulation potential of ?0.25 V, a scan rate of 5 mV. s^?1, a pulse height of 25 mV, and a differential pulse scan mode. The response of 9‐phenanthrol is linear over the concentration range 1.0–12.0 ppb. For an accumulation time of 5 minutes, the detection limit was found to be 0.2 ppb (1.03×10^?9 M). The more convenient relation to measure the 9‐phenanthrol in the presence of copper and other metals was also investigated. The utility of the method was demonstrated by the presence of 9‐phenanthrol in samples of sea water and human urine. Cyclic voltammetry was used to characterize the interfacial and redox behavior.     

Overlapping voltammetric peaks—an analytical procedure for simultaneous determination of trace metals. Application to food and environmental matrices

Voltammetric methods are very suitable, versatile and rapid techniques for simultaneous determination of metals in complex matrices. The present work, determination of Cu(II), Sn(II), Sb(III), Tl(I), and Pb(II) by square-wave anodic-stripping voltammetry and Cr(VI) by square-wave adsorptive-stripping voltammetry, is an interesting example of the possibility of simultaneous determination of each single element in food and environmental samples, even in the presence of reciprocal interference. Dibasic ammonium citrate, pH 6.3 or 8.2, was employed as supporting electrolyte. The voltammetric measurements were carried out using a stationary hanging mercury drop electrode as working electrode and a platinum electrode and an Ag|AgCl|KCl_sat electrode as auxiliary and reference electrodes, respectively. The analytical procedure was verified by analysis of standard reference materials—wholemeal BCR-CRM 189, wheat flour NIST-SRM 1567a, rice flour NIST-SRM 1568a, estuarine sediment BCR-CRM 277, river sediment BCR-CRM 320, and Montana soil with moderately elevated traces NIST-SRM 2711. Precision and accuracy, expressed as relative standard deviation and relative error, respectively, were generally below 6% whereas limits of detection for each element were below 0.069 g g^–1. In the presence of reciprocal interference the standard addition method considerably improved the resolution of the voltammetric technique, even for very high element concentration ratios. After being set up on the standard reference materials the analytical procedure was transferred and applied to commercial samples of meal and soil samples taken from sites devoted to agricultural practice. A critical comparison with graphite furnace atomic-absorption spectroscopy is also discussed. Work partially presented at Euroanalysis XIII, Salamanca, Spain, 5–10 September 2004     

Convenient Method for Reduction of C-N Double Bonds in Oximes,Imines, and Hydrazones Using Sodium Borohydride–Raney Ni System

A practical method has been developed for reduction of C-N double bond in oximes, imines, and hydrazones with sodium borohydride catalyzed by Raney Ni. The reactions were carried out in basic aqueous solution, and the desired products were obtained in moderate yields after a simple procedure. This method can be applied to synthesize simpler aliphatic or aromatic amines and its analogs.     

Synthesis of 7,7’-Disubstituted BINAP and Their Application in Asymmetric Catalytic Reaction

The design of new chiral ligands plays a very important role in the development of transition metal catalyzed asymmetric synthesis. Many chiral diphosphine ligands have been prepared and applied in asymmetric catalytic reactions with excellent enantioselectivities. Among the chiral diphosphine ligands reported, BINAP was found to have been the widest application in the transition metal catalyzed reaction. Recently we have developed a novel oxovanadium (Ⅳ) complex catalyst for the oxidative …     

Application of multilayered strategy for variable selection in QSAR modeling of PET and SPECT imaging agents as diagnostic agents for Alzheimer’s disease

Structural Chemistry - Non-invasive imaging of amyloid beta (Aβ) and tau fibrils in the brain may support an early and precise diagnosis of Alzheimer’s disease. Molecular imaging...     

Application of β-cyclodextrin in polymeric solid phase for separation and determination of lead in different environmental matrices

Immobilization of β-cyclodextrin on Dowex resin as an insoluble polymeric matrix by covalent bond presents a new solid-phase medium for preconcentration of Pb (II) at trace level in environmental samples prior to its flame atomic absorption spectrometric determination. The method is based on the sorption of lead after passing on modified Dowex sorbent in a column. The effect of several parameters such as pH, flow rate of sample, eluent kind and volume was investigated. The sorption capacity of the matrix has been found to be 0.4996?mg?g^?1 of adsorbent with the preconcentration factor of 250 for Pb (II). Nitric acid (3 M) as an eluent was sufficient to obtain quantitative recovery (>95%) for Pb (II). The optimum flow rate was 10?ml?min ^?1. The calibration curve was linear in the range of (3–250?ng?mL^?1) with a correlation coefficient of 0.9995. The limit of detection (LOD) based on three times the standard deviation of the blank was 1.37?ng?mL^?1. The relative standard deviation (RSD) for determination of 10?ng?mL^?1 and 100?ngmL^?1 of Pb (II) was 3.00 % and 0.58 % (n?=?10), respectively. The method was successfully applied to determination of lead in some environmental samples such as tap water, river water, soil and rice.