The voltammetric behaviour of three 5-nitroimidazoles,metronidazole,tinidazole and ornidazole,was investigated,and a method was developed for the simultaneous determination of these compounds,based on their reduction ...The voltammetric behaviour of three 5-nitroimidazoles,metronidazole,tinidazole and ornidazole,was investigated,and a method was developed for the simultaneous determination of these compounds,based on their reduction at a hanging mercury drop electrode（HMDE） in pH 8.95 buffer with differential pulse voltammetric（DPV） approach.Well defined voltammetric waves with peak potentials of -692,-640 and -652 mV were observed for these compounds,respectively.It is difficult to determine them individually from their mixtures without preseparation,for their voltammetric peaks overlapped seriously,so the chemometrics were used to resolve the overlapped voltammogram and quantify the mixtures.The proposed method was successfully applied to the determination of three 5-nitroimidazoles in milk and honey samples.展开更多
New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation o...New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse modulation.The optimum conditions for the analysis of morphine are pH 10.5,Eacc of -100 mV（vs.Ag/AgCl）,and tacc of 120 s.The peak current is proportional to the concentration of morphine,and a Linear calibration graph is obtained at 0.01-3.10μg mL^-1.A relative standard deviation of 1.06%（n=5）was obtained,and the limit of detection was 3 ng mL^-1.The capabiLity of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.展开更多
A DNA biosensor with [Ru（DA-bpy）3]Cl2（DA-bpy：4,4＇-diamino-2,2＇-bipyridine） （RuL） as the electrochemical probe was prepared on pyrolytic graphite electrode （PGE） through the supramolecular interaction betwee...A DNA biosensor with [Ru（DA-bpy）3]Cl2（DA-bpy：4,4＇-diamino-2,2＇-bipyridine） （RuL） as the electrochemical probe was prepared on pyrolytic graphite electrode （PGE） through the supramolecular interaction between RuL complex and DNA template. Cyclic voltammetry of RuL-DNA film showed a pair of stable and reversible peaks corresponding to the Ru（Ⅲ）/Ru（Ⅲ） redox potential of-0.165 V versus AglAgCl in pa 7.4 0.1 mol·L^-1Tris-HCl. The electron transfer was expected across the double-strand DNA by an ＂electron tunneling＂ mechanism. When the DNA biosensor was immerged in gold （Ⅲ） buffer solution, the current peak signal （I） of the RuL-DNA supramolecular depressed and △I was linear in the concentration range of Au ion from 1×10^-7 to 2×10^-5 mol·L^-1 with a regression coefficient of 0.9879. The detection limit was 5×10^-8 mol·L^-1. The developed procedures were applied to the analysis of synthetic samples of real materials with good sensitivity and selectivity.展开更多
A reliable method for simultaneous determination of three antibiotic drugs（levofloxacin,gatifloxacin and lomefloxacin） by differential pulse stripping voltammetry（DPSV） in Britton-Robinson buffer（pH 7.96） was pr...A reliable method for simultaneous determination of three antibiotic drugs（levofloxacin,gatifloxacin and lomefloxacin） by differential pulse stripping voltammetry（DPSV） in Britton-Robinson buffer（pH 7.96） was presented.The method is based on adsorptive accumulation of the antibacterial drugs on a hanging mercury dropping electrode（HMDE）,followed by the reduction of the adsorptive species by the technique of DPSV.Optimal conditions,the deposition time of 80 s,the deposition potential of—1250 mV,and the scan rate of 25 mV/s,were obtained.The linear concentration ranges of 0.010-0.080μg/mL were obtained for all these three antibiotic drugs,while the detection limits were 2.38,3.20 and 1.60ng/mL for levofloxacin,gatifloxacin and lomefloxacin,respectively.In this work,chemometrics methods,such as classical least squares（CLS）,partial least squares（PLS）, principle component regression（PCR） and radial basis function-artificial neural networks（RBF-ANN）,were used to quantitatively resolve the overlapping signals.It was found that PCR gave the best results with total relative prediction error（RPE_T） of 7.71%.The proposed method was applied to determine these three drugs in several commercial food samples with spiked method and yielded satisfactory recoveries.展开更多
Differential pulse voltammetry(DPV) was applied to the determination of alkaline phosphatase(ALP) activity in human serum with phenyl phosphate as the substrate. Phenyl phosphate can enzymatically be hydrolyzed to pro...Differential pulse voltammetry(DPV) was applied to the determination of alkaline phosphatase(ALP) activity in human serum with phenyl phosphate as the substrate. Phenyl phosphate can enzymatically be hydrolyzed to produce phenol which is quantified by DPV at +660 mV(vs.Ag/AgCl) in the concentration range of 2.0_100 μmol/L. The standard curve for ALP is linear over the range from 0.06 to 1000 U/L with a relative standard deviation of 3.0%. The conditions for the enzymatic reaction and voltammetric detection were optimized and the kinetic constants were also examined.The human serum samples were tested by this method and the results were in good agreement with those obtained by the routine p-nitrophenyl phosphate spectrophotometric method.展开更多
A PCV-modified electrode was simply prepared by dip-coating a pyrolytic graphite electrode in a NaAc-HAc buffer solution of PCV. The peak currents of differential pulse voltammograms (DPV) decrease with the addition o...A PCV-modified electrode was simply prepared by dip-coating a pyrolytic graphite electrode in a NaAc-HAc buffer solution of PCV. The peak currents of differential pulse voltammograms (DPV) decrease with the addition of Al and the peak potentials remain the same. The decreasing of Delta i(p) is linear with Al concentration in the range of 1 x 10(-8) similar to 1 x 10(-7) mol/L. The detection limit is 5 x 10(-9) mol/L and the relative standard deviation for 4 x 10(-8) mol/L Al is 2.9% (n=8). No serious interference was found. The determination of Al in water samples is reported.展开更多
A new method was proposed for study of organic reducing substances in soils. According to the theoretical relationship between the voltammetric behaviors and reduction-oxidation reaction of reducing substances, the wo...A new method was proposed for study of organic reducing substances in soils. According to the theoretical relationship between the voltammetric behaviors and reduction-oxidation reaction of reducing substances, the working conditions of differential pulse voltammetry (d.p. v.) for determining the organic reducing substances produced during the processes of the anaerobic decomposition of plant materials were established with a glass carbon electrode as working electrode, 1 M Ag-AgCl electrode with large area as reference electrode, 0.2 M NH4AC as supporting electrolyte and pH buffer solution, pulse amplitude (AE) of 25 mV, scan rate at 2 mV·S-1and scan potential ranging from -0.5 to +1.2 voltage(vs. M Ag-AgCl). The peak current proportional to the concentration of reducing substances, and the characteristic peak potential of each organic reducing substance were regarded as the quantitative and qualitative base, respectively. These results obtained under the conditions mentioned above directly reflect both the reducing intensity and capacity of the organic reducing system in soils.展开更多
A differential pulse voltammetric method was developed for the sensitive andselective determination of Cu(II) at 4-methoxy-2,6-bis(3,5-dimethylpyrazoyl)-l,3,5-triazine modifiedcarbon paste electrode in 0.05 mol/L KHC_...A differential pulse voltammetric method was developed for the sensitive andselective determination of Cu(II) at 4-methoxy-2,6-bis(3,5-dimethylpyrazoyl)-l,3,5-triazine modifiedcarbon paste electrode in 0.05 mol/L KHC_8H_4O_4 solution (pH = 4.02). The oxidation peak of Cu(II)was observed at 0.065 V(vs Ag/AgCl) by scanning the potential in positive direction. The analysisprocedure consisted of an open circuit accumulation step in stirred sample solution. It was followedby medium exchange to a clean solution and subsequently an anodic potential scan was affected toobtain the voltammetric peak. The current was proportional to the concentration of the Cu(II) ion ina range of 1 X 10^(-7) -1 X 10^(-4) mol/L for 6 min accumulation; the most of metal ions did notinterfere with the determination. The developed method was applied to Cu (II) determination incoal-ash sample, the results agreed with that of atomic adsorption spectroscopy (AAS).展开更多
This article describes the use of a boron-doped diamond electrode (BDDE) as an electrochemical sensor for the simultaneous determination of omnipaque (OMP) and paracetamol (PCM) in perchloric acid medium (HClO4 0.1 M)...This article describes the use of a boron-doped diamond electrode (BDDE) as an electrochemical sensor for the simultaneous determination of omnipaque (OMP) and paracetamol (PCM) in perchloric acid medium (HClO4 0.1 M) and in complex matrices such as tomato, carrot and cucumber juices and waste water from the Treichville University Hospital. Voltammetric studies allowed us to have well-defined oxidation peaks at distinct potentials of OMP (E = 0.5 V/SCE) and PCM (E = 0.7 V/SCE). Under optimized conditions, well-defined quantities of OMP and PCM, introduced simultaneously by metered additions, gave linear responses in concentration ranges of 259.8 - 467.2 μM for OMP and 58.73 - 116.3 μM PCM. The detection limits obtained are 7.23 μΜ and 3.6 μΜ respectively for OMP and PCM with recovery rates between 85.8% ± 0.1% and 92.6% ± 0.1% for OMP and between 99.9% ± 0.1% and 101.2% ± 0.4% for the PCM. This technique has been successfully used to simultaneously detect these pharmaceuticals in these complex environments. It allows recovery of OMP and PCM respectively up to 97.5% ± 0.0% and 91.6% ± 0.3% in tomato juice;100.0% ± 0.0% and 95.2% ± 0.2% in carrot juice;101.4% ± 0.1% and 97.3% ± 0.3% in cucumber juice;100.1% ± 0.9% and 100.9% ± 0.1% in wastewater. The relevance of this technique for the simultaneous detection of OMP and PCM in tomato, carrot, cucumber juices and in waste water can be studied in the context of the contamination of certain fruits and vegetables by the substances organic pharmaceuticals released into the environment without prior treatment.展开更多
Vitamin B12 is a type of vitamin also known by the name cobalamin. B12 is involved in many metabolism activities, including DNA synthesis, nervous system, red blood formation and immune system. Therefore, we chose the...Vitamin B12 is a type of vitamin also known by the name cobalamin. B12 is involved in many metabolism activities, including DNA synthesis, nervous system, red blood formation and immune system. Therefore, we chose the Differential Pulse Polarography (DPP) method is that has a high sensitivity for the determination of vitamin B12. This determination was possible with cobalt present in vitamin B12 structure. Since Co(III) is formed from the oxidation of the vitamin, its polarographic behavior had to be determined in various electrolytes such as acetate, borate, phosphate and ammonia. The polarograms of Co(III) were taken in these electrolytes in which 1.0 M NH3/ (pH = 9.8) and 1.0 M AcOH/AcO- (pH = 4.0) were found as the most suitable electrolytes. This method was successfully applied vitamin of B12 determination in a 1 mL ampoule with high precision. The LOD was found as 3.7 × 10-7 for instead of (S/N = 3). Besides Co(III), interference effects of Zn(II), Ni(II), Cr(III), Fe(III), Cu(II), Cd(II) and Se(IV) were also studied. It was found that only Zn(II) peak had an overlap Co(III) peak in ammonium buffer. This problem could be solved by working in 1.0 M AcOH/AcO- (pH = 4.0) buffer. B12, which is 1000 μg in 1 mL vitamin ampoule, was found for 4 measurements as 999 ± 15 μg as a result of 95% confidence interval.展开更多
During direct chilling(DC)casting of ZK61 alloys,the primary and secondary cooling causes strong thermal gradients,which leads to the uneven crystallization rate and thermal contraction in different positions of the i...During direct chilling(DC)casting of ZK61 alloys,the primary and secondary cooling causes strong thermal gradients,which leads to the uneven crystallization rate and thermal contraction in different positions of the ingot.The consequences manifested appearance of heterogeneous grains,huge casting stresses,and even hot cracking flaws.In this paper,chemical and physical methods were integrated to produce large-scale magnesium(Mg)alloy ingots.A φ525 mm ZK61-RE alloy ingot that was refined,homogeneous,and free from hot cracking was obtained via the DC process coupled with a differential low frequency pulsed magnetic field(DLPM).The effects of rare earth(RE)and DLPM on the hot cracking tendency were investigated,and the mechanism of hot cracking formation and modification in largescale ingots was revealed.The findings indicate that the addition of moderate amounts of RE lessens the tendency of hot cracking in large-scale ZK61 alloy ingots.This is mainly attributed to the addition of RE increases the content of the second phase,thus enhancing the ability of the eutectic liquid phase to feed the cracking.With the introduction of DLPM,the grain sizes are significantly refined and homogenized,and there is no obvious hot cracking observed in the ingot.This is because the coupling of the DLPM provides a more homogeneous temperature field,leading to the synchronization of the solidification process,and the consequent reduction of the casting stress,thus reducing the driving force for the formation of hot cracking.In addition,the casting conditions are modified to enhance the ability of solidification feeding and the resistance to hot cracking.This work provides theoretical and practical references for the preparation of large-scale high-quality Mg alloy ingots.展开更多
In this work,we reported a simultaneous determination approach for Pb(II),Cd(II)and Zn(II)atμg L 1concentration levels using differential pulse stripping voltammetry on a bismuth film electrode(BiFE).The BiFE could b...In this work,we reported a simultaneous determination approach for Pb(II),Cd(II)and Zn(II)atμg L 1concentration levels using differential pulse stripping voltammetry on a bismuth film electrode(BiFE).The BiFE could be prepared in situ when the sample solution contained a suitable amount of Bi(NO)3,and its analytical performance was evaluated for the simultaneous determination of Pb(II),Cd(II)and Zn(II)in solutions.The determination limits were found to be 0.19μg L 1for Zn(II),and0.28μg L 1for Pb(II)and Cd(II),with a preconcentration time of 300 s.The BiFE approach was successfully applied to determine Pb(II),Cd(II)and Zn(II)in tea leaf and infusion samples,and the results were in agreement with those obtained using an atomic absorption spectrometry approach.Without Hg usage,the in situ preparation for BiFE supplied a green and acceptability sensitive method for the determination of the heavy metal ions.展开更多
An electrochemical flow device has been developed for the determination of heavy metal ions(HMI)in water using multiwalled carbon nanotubes(MWCNTs)/Nafion(NA)/Hg electrode,by mean of diff erential pulse anodic strippi...An electrochemical flow device has been developed for the determination of heavy metal ions(HMI)in water using multiwalled carbon nanotubes(MWCNTs)/Nafion(NA)/Hg electrode,by mean of diff erential pulse anodic stripping voltammetry coupled with sequential injection analysis.The accuracy of the determination was ensured by the great electrical conductivity of MWCNTs and the high adsorption capacity of Hg.NA was used for MWCNTs immobilization for the long-term application of the electrode.The mercury film was cleaned after determination and another one would form during deposition.A lower limit of detection and a wider determination range of Cd^(2+)and Pb^(2+)could be achieved using the automatically analytical device combining with the MWCNTs/NA/Hg-modified electrode.The real-time monitoring of Cd^(2+)and Pb^(2+)in fresh water using this device continued for 10 days.The results indicated that the method was potential for on-site and real-time determination of HMI in water samples.展开更多
A novel differential pulse anodic stripping voltammetry for the determination of trace amounts of lead, using a biomacromolecule heparin drop-coated modified glassy carbon electrode, has been described. Pb2+ was depos...A novel differential pulse anodic stripping voltammetry for the determination of trace amounts of lead, using a biomacromolecule heparin drop-coated modified glassy carbon electrode, has been described. Pb2+ was deposited on the surface of a heparin-modified electrode at -1.0 V (vs. SCE) via forming Pb2+-heparin and subsequent re-duction at the electrode. In the following step, Pb-heparin was oxidized, and voltammograms were recorded by scanning the potential in a positive direction. Conditions were optimized with respect to the pH of the medium, the mass of drop-coated heparin, accumulation potential and accumulation time. The peak current was proportional to the Pb2+ concentration in the range of 2.0×10-9 to 7.0×10-7 mol/L. The detection limit was 3.0×10-10 mol/L. The relative standard deviation was 4.83% for 1.0×10-8 mol / L Pb2+ (n=10). The developed method has been applied to the determination of Pb2+ in water samples with satisfactory results.展开更多
The determination of trace element Pb in electrolyte MnSO_4H_2SO_4 was studied with differential pulse po-larography. The trace Pb was originated from new type Pb-Ag-Ca alloy anode being used in preduction processof e...The determination of trace element Pb in electrolyte MnSO_4H_2SO_4 was studied with differential pulse po-larography. The trace Pb was originated from new type Pb-Ag-Ca alloy anode being used in preduction processof electrolytic MnO_2 (EMD). The KCl was added as background of electrolyte. The differential pulse polarco-gram obtained for Pb(Ⅱ) is well in peak contour and is easy to determination. The peak potential is -0. 44 V(vs Ag-AgCl potential , experimental valuel). The Pb content may be determined by standard addition methodwhich is simple , reliable and fast. This study presents some foundamental data for Pb-Ag-Ca anode (abbreviated to PAC anede). The consuming rate for PAC anode is evaluated as 4. 82% annually.展开更多
The second derivative differential pulse polarography was developed for the quantitative determination of active principles in medicinal herbs (baicalin in Scutellaria baicalensis Georgi, indigo in Baphicacanthus cusi...The second derivative differential pulse polarography was developed for the quantitative determination of active principles in medicinal herbs (baicalin in Scutellaria baicalensis Georgi, indigo in Baphicacanthus cusia (Nees) Bremek, paeonol in Paeonia suffruticosa Andr and piperine in Piper longum L ) The C O group in baicalin, indigo, paeonol and piperine could be reduced to CH OH in acidic solution at the dropping mercury electrode, and showed very good second derivative differential pulse polarographic peak at 1 550V, 1 300V, 1 630V and 0 860V (vs Ag/AgCl) respectively The linear relationship between concentration of baicalin, indigo, paeonol, piperine and peak height was obtained in the concentration range of 4 5×10 5 ～ 2 7×10 4 mol·L 1 , 3 8×10 5 ～ 4 2×10 4 mol·L 1 , 1 0～6 0×10 4 mol·L 1 and 7 0×10 5 ～2 5×10 4 mol·L 1 and the determination limits were 9 0×10 8 mol·L 1 , 8 4×10 9 mol·L 1 , 9 2×10 9 mol·L 1 and 8 7×10 9 mol·L 1 respectively This method is simple, rapid and sensitive, and the results are accurate展开更多
The potassium phosphate buffer as a supporting electrolyte of anticancer drug(5-fluorouracil(5-FU))was the best among solutions of sodium phosphate buffer and Britton Robinson buffer in differential pulse polarography...The potassium phosphate buffer as a supporting electrolyte of anticancer drug(5-fluorouracil(5-FU))was the best among solutions of sodium phosphate buffer and Britton Robinson buffer in differential pulse polarography(DPP)at pH=7.0 and T=37℃.The changes of temperature did not effect on inactivity of the supporting electrolyte(potassium phosphate buffer at T=10-50℃),and pH of the solution did not exceed 2%of each 5℃(at pH=7.0,by modified thermostat cell).However,the frequency measurements showed clear effect of temperature on diffusion current(IP/μA)of the chemotherapy compound in the range of 20-50℃and under primary conditions.Then,the polarography measurements of 5-FU drug(at 10μM,pH=7 and T=37℃)gradually led to the optimum conditions:deposition potential=-0.9 V;drop size=9.0 mm^(3);deposition time=15.0 s;equilibration time=5.0 s;pulse amplitude=100 mV;pulse time=7.0 ms;voltage step=6 mV;voltage step time=0.3 s;and sweep rate=20.0 mV/s.The thermal assessment of 5-FU drug(after achievement of the optimum conditions)in a new thermostat vessel at HMDE by DPP showed that the reaction of 5-FU molecules represented pseudo first order reaction,instead of first order;the secondary waves of 5-FU drug may be due to formation of molecular complexes in aqueous solution and the reduction of 5-FU molecules at mercury surface electrode appeared as physisorption,instead of chemisorption.展开更多
The determination of trace rhenium(Ⅶ)by differential pulse polarography in the system of H_2SO_4-(NH_2OH)_2·H_2SO_4-TeO_4^(2-) is markedly improved by the addition of Nitron,which is adsorbed on the surface of m...The determination of trace rhenium(Ⅶ)by differential pulse polarography in the system of H_2SO_4-(NH_2OH)_2·H_2SO_4-TeO_4^(2-) is markedly improved by the addition of Nitron,which is adsorbed on the surface of mercury electrode.The limit of detection is down to 2×10^(-10) M.The adsorptive peak potential is -0.80V(vs.SCE).In the ranges of 5×10^(-10)-10^(-8),1×10^(-8)-10^(-7) and 1× 10^(-7)-10^(-6)M,there are good linear relationships between the peak current increment and the concentration,of which the relative standard deviations are 9.5,6.6,1.8% respectively with the correlation coefficients of linear regression of 0.995—0.999.The results relating to this polarographic wave show that it is an adsorption-catalytic wave.The mechanism of the electrode reaction is dis- cussed.展开更多
Even in small concentrations,toxic metals like lead,cadmium,and mercury are dangerous to the environment and human health.Environmental monitoring depends on precisely identifying these heavy metals,particularly cadmi...Even in small concentrations,toxic metals like lead,cadmium,and mercury are dangerous to the environment and human health.Environmental monitoring depends on precisely identifying these heavy metals,particularly cadmium ions(Cd(Ⅱ)).In this study,we present a novel screen-printed carbon electrode(SPCE)modified with single crystallineα-Fe_(2)O_(3)nano-hexagons that functions as a sensor for detecting Cd(Ⅱ).The performance of the fabricated sensor was thoroughly assessed and compared with unmodified SPCE using the voltammetric method.The crystalline structure of the synthesizedα-Fe_(2)O_(3)nano-hexagons was confirmed through XRD,and surface analysis revealed an average diameter and thickness of 86 nm and 9 nm,respectively.Theα-Fe_(2)O_(3)modified SPCE yields a 7-fold enhanced response(at pH 5.0 vs.Ag/AgCl)to Cd(Ⅱ)than bare SPCE.The modified electrode effectively detects Cd(Ⅱ)with a linear response range of up to 333.0μmol/L and a detection limit of 0.65 nmol/L under ideal circumstances.This newly fabricated sensor offers significant potential for environmental monitoring applications by providing outstanding practicality,anti-interference ability,and repeatability for detecting Cd(Ⅱ)in water samples.展开更多
The design and implementation of a novel ADC architecture called ring-ADC for digital voltage regulator module controllers are presented. Based on the principle of voltage-controlled oscillators＇ transform from volta...The design and implementation of a novel ADC architecture called ring-ADC for digital voltage regulator module controllers are presented. Based on the principle of voltage-controlled oscillators＇ transform from voltage to frequency,the A/D conversion of ring-ADC achieves good linearity and precise calibration against process variations compared with the delay-line ADC. A differential pulse counting discriminator also helps decrease the power consumption of the ring-ADC. It is fabricated with a Chartered 0.35μm CMOS process, and the measurement results of the integral and differential nonlinearity performance are 0.92LSB and 1.2LSB respectively. The maximum gain error measured in ten sample chips is ± 3.85%. With sampling rate of 500kHz and when the voltage regulator module （VRM） works in steady state, the ring-ADC＇s average power consumption is 2.56mW. The ring-ADC is verified to meet the requirements for digital VRM controller application.展开更多
文摘The voltammetric behaviour of three 5-nitroimidazoles,metronidazole,tinidazole and ornidazole,was investigated,and a method was developed for the simultaneous determination of these compounds,based on their reduction at a hanging mercury drop electrode（HMDE） in pH 8.95 buffer with differential pulse voltammetric（DPV） approach.Well defined voltammetric waves with peak potentials of -692,-640 and -652 mV were observed for these compounds,respectively.It is difficult to determine them individually from their mixtures without preseparation,for their voltammetric peaks overlapped seriously,so the chemometrics were used to resolve the overlapped voltammogram and quantify the mixtures.The proposed method was successfully applied to the determination of three 5-nitroimidazoles in milk and honey samples.
文摘New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse modulation.The optimum conditions for the analysis of morphine are pH 10.5,Eacc of -100 mV（vs.Ag/AgCl）,and tacc of 120 s.The peak current is proportional to the concentration of morphine,and a Linear calibration graph is obtained at 0.01-3.10μg mL^-1.A relative standard deviation of 1.06%（n=5）was obtained,and the limit of detection was 3 ng mL^-1.The capabiLity of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.
基金This study is financially supported by the National Natural Science Foundation of China (No. 60508012)the Natural Sci-ence Foundation of Zhejiang Province (No. Y106725)+1 种基金the Natural Science Foundation of Ningbo (No. 2006A610048)the Scientific and Technological Project Funding of Zhejiang Province (No. 2006C31040).
文摘A DNA biosensor with [Ru（DA-bpy）3]Cl2（DA-bpy：4,4＇-diamino-2,2＇-bipyridine） （RuL） as the electrochemical probe was prepared on pyrolytic graphite electrode （PGE） through the supramolecular interaction between RuL complex and DNA template. Cyclic voltammetry of RuL-DNA film showed a pair of stable and reversible peaks corresponding to the Ru（Ⅲ）/Ru（Ⅲ） redox potential of-0.165 V versus AglAgCl in pa 7.4 0.1 mol·L^-1Tris-HCl. The electron transfer was expected across the double-strand DNA by an ＂electron tunneling＂ mechanism. When the DNA biosensor was immerged in gold （Ⅲ） buffer solution, the current peak signal （I） of the RuL-DNA supramolecular depressed and △I was linear in the concentration range of Au ion from 1×10^-7 to 2×10^-5 mol·L^-1 with a regression coefficient of 0.9879. The detection limit was 5×10^-8 mol·L^-1. The developed procedures were applied to the analysis of synthetic samples of real materials with good sensitivity and selectivity.
基金support by the National Natural Science Foundation of China (No21065007)the State Key Laboratory of Food Science and Technology of Nanchang University(SKLF-MB-201002 and SKLF-TS-200919)
文摘A reliable method for simultaneous determination of three antibiotic drugs（levofloxacin,gatifloxacin and lomefloxacin） by differential pulse stripping voltammetry（DPSV） in Britton-Robinson buffer（pH 7.96） was presented.The method is based on adsorptive accumulation of the antibacterial drugs on a hanging mercury dropping electrode（HMDE）,followed by the reduction of the adsorptive species by the technique of DPSV.Optimal conditions,the deposition time of 80 s,the deposition potential of—1250 mV,and the scan rate of 25 mV/s,were obtained.The linear concentration ranges of 0.010-0.080μg/mL were obtained for all these three antibiotic drugs,while the detection limits were 2.38,3.20 and 1.60ng/mL for levofloxacin,gatifloxacin and lomefloxacin,respectively.In this work,chemometrics methods,such as classical least squares（CLS）,partial least squares（PLS）, principle component regression（PCR） and radial basis function-artificial neural networks（RBF-ANN）,were used to quantitatively resolve the overlapping signals.It was found that PCR gave the best results with total relative prediction error（RPE_T） of 7.71%.The proposed method was applied to determine these three drugs in several commercial food samples with spiked method and yielded satisfactory recoveries.
基金the National Natural Science Foundation of China(No.2 0 0 75 0 13) and China Postdoctoral Science Foun-dation(No.2 0 0 30 33492 )
文摘Differential pulse voltammetry(DPV) was applied to the determination of alkaline phosphatase(ALP) activity in human serum with phenyl phosphate as the substrate. Phenyl phosphate can enzymatically be hydrolyzed to produce phenol which is quantified by DPV at +660 mV(vs.Ag/AgCl) in the concentration range of 2.0_100 μmol/L. The standard curve for ALP is linear over the range from 0.06 to 1000 U/L with a relative standard deviation of 3.0%. The conditions for the enzymatic reaction and voltammetric detection were optimized and the kinetic constants were also examined.The human serum samples were tested by this method and the results were in good agreement with those obtained by the routine p-nitrophenyl phosphate spectrophotometric method.
文摘A PCV-modified electrode was simply prepared by dip-coating a pyrolytic graphite electrode in a NaAc-HAc buffer solution of PCV. The peak currents of differential pulse voltammograms (DPV) decrease with the addition of Al and the peak potentials remain the same. The decreasing of Delta i(p) is linear with Al concentration in the range of 1 x 10(-8) similar to 1 x 10(-7) mol/L. The detection limit is 5 x 10(-9) mol/L and the relative standard deviation for 4 x 10(-8) mol/L Al is 2.9% (n=8). No serious interference was found. The determination of Al in water samples is reported.
文摘A new method was proposed for study of organic reducing substances in soils. According to the theoretical relationship between the voltammetric behaviors and reduction-oxidation reaction of reducing substances, the working conditions of differential pulse voltammetry (d.p. v.) for determining the organic reducing substances produced during the processes of the anaerobic decomposition of plant materials were established with a glass carbon electrode as working electrode, 1 M Ag-AgCl electrode with large area as reference electrode, 0.2 M NH4AC as supporting electrolyte and pH buffer solution, pulse amplitude (AE) of 25 mV, scan rate at 2 mV·S-1and scan potential ranging from -0.5 to +1.2 voltage(vs. M Ag-AgCl). The peak current proportional to the concentration of reducing substances, and the characteristic peak potential of each organic reducing substance were regarded as the quantitative and qualitative base, respectively. These results obtained under the conditions mentioned above directly reflect both the reducing intensity and capacity of the organic reducing system in soils.
文摘A differential pulse voltammetric method was developed for the sensitive andselective determination of Cu(II) at 4-methoxy-2,6-bis(3,5-dimethylpyrazoyl)-l,3,5-triazine modifiedcarbon paste electrode in 0.05 mol/L KHC_8H_4O_4 solution (pH = 4.02). The oxidation peak of Cu(II)was observed at 0.065 V(vs Ag/AgCl) by scanning the potential in positive direction. The analysisprocedure consisted of an open circuit accumulation step in stirred sample solution. It was followedby medium exchange to a clean solution and subsequently an anodic potential scan was affected toobtain the voltammetric peak. The current was proportional to the concentration of the Cu(II) ion ina range of 1 X 10^(-7) -1 X 10^(-4) mol/L for 6 min accumulation; the most of metal ions did notinterfere with the determination. The developed method was applied to Cu (II) determination incoal-ash sample, the results agreed with that of atomic adsorption spectroscopy (AAS).
文摘This article describes the use of a boron-doped diamond electrode (BDDE) as an electrochemical sensor for the simultaneous determination of omnipaque (OMP) and paracetamol (PCM) in perchloric acid medium (HClO4 0.1 M) and in complex matrices such as tomato, carrot and cucumber juices and waste water from the Treichville University Hospital. Voltammetric studies allowed us to have well-defined oxidation peaks at distinct potentials of OMP (E = 0.5 V/SCE) and PCM (E = 0.7 V/SCE). Under optimized conditions, well-defined quantities of OMP and PCM, introduced simultaneously by metered additions, gave linear responses in concentration ranges of 259.8 - 467.2 μM for OMP and 58.73 - 116.3 μM PCM. The detection limits obtained are 7.23 μΜ and 3.6 μΜ respectively for OMP and PCM with recovery rates between 85.8% ± 0.1% and 92.6% ± 0.1% for OMP and between 99.9% ± 0.1% and 101.2% ± 0.4% for the PCM. This technique has been successfully used to simultaneously detect these pharmaceuticals in these complex environments. It allows recovery of OMP and PCM respectively up to 97.5% ± 0.0% and 91.6% ± 0.3% in tomato juice;100.0% ± 0.0% and 95.2% ± 0.2% in carrot juice;101.4% ± 0.1% and 97.3% ± 0.3% in cucumber juice;100.1% ± 0.9% and 100.9% ± 0.1% in wastewater. The relevance of this technique for the simultaneous detection of OMP and PCM in tomato, carrot, cucumber juices and in waste water can be studied in the context of the contamination of certain fruits and vegetables by the substances organic pharmaceuticals released into the environment without prior treatment.
基金the Gazi University research fund for the financial support of this research.
文摘Vitamin B12 is a type of vitamin also known by the name cobalamin. B12 is involved in many metabolism activities, including DNA synthesis, nervous system, red blood formation and immune system. Therefore, we chose the Differential Pulse Polarography (DPP) method is that has a high sensitivity for the determination of vitamin B12. This determination was possible with cobalt present in vitamin B12 structure. Since Co(III) is formed from the oxidation of the vitamin, its polarographic behavior had to be determined in various electrolytes such as acetate, borate, phosphate and ammonia. The polarograms of Co(III) were taken in these electrolytes in which 1.0 M NH3/ (pH = 9.8) and 1.0 M AcOH/AcO- (pH = 4.0) were found as the most suitable electrolytes. This method was successfully applied vitamin of B12 determination in a 1 mL ampoule with high precision. The LOD was found as 3.7 × 10-7 for instead of (S/N = 3). Besides Co(III), interference effects of Zn(II), Ni(II), Cr(III), Fe(III), Cu(II), Cd(II) and Se(IV) were also studied. It was found that only Zn(II) peak had an overlap Co(III) peak in ammonium buffer. This problem could be solved by working in 1.0 M AcOH/AcO- (pH = 4.0) buffer. B12, which is 1000 μg in 1 mL vitamin ampoule, was found for 4 measurements as 999 ± 15 μg as a result of 95% confidence interval.
基金Project supported by the Jiangxi Province Key Laboratory of Light Alloy(2024SSY05031)the National Natural Science Foundation of China(52061028)+1 种基金the National Key Research and Development Program of China(2021YFB3501001)the Major Research and Development Projects of Jiangxi Province(20223BBE51021,20213AAE02014)。
文摘During direct chilling(DC)casting of ZK61 alloys,the primary and secondary cooling causes strong thermal gradients,which leads to the uneven crystallization rate and thermal contraction in different positions of the ingot.The consequences manifested appearance of heterogeneous grains,huge casting stresses,and even hot cracking flaws.In this paper,chemical and physical methods were integrated to produce large-scale magnesium(Mg)alloy ingots.A φ525 mm ZK61-RE alloy ingot that was refined,homogeneous,and free from hot cracking was obtained via the DC process coupled with a differential low frequency pulsed magnetic field(DLPM).The effects of rare earth(RE)and DLPM on the hot cracking tendency were investigated,and the mechanism of hot cracking formation and modification in largescale ingots was revealed.The findings indicate that the addition of moderate amounts of RE lessens the tendency of hot cracking in large-scale ZK61 alloy ingots.This is mainly attributed to the addition of RE increases the content of the second phase,thus enhancing the ability of the eutectic liquid phase to feed the cracking.With the introduction of DLPM,the grain sizes are significantly refined and homogenized,and there is no obvious hot cracking observed in the ingot.This is because the coupling of the DLPM provides a more homogeneous temperature field,leading to the synchronization of the solidification process,and the consequent reduction of the casting stress,thus reducing the driving force for the formation of hot cracking.In addition,the casting conditions are modified to enhance the ability of solidification feeding and the resistance to hot cracking.This work provides theoretical and practical references for the preparation of large-scale high-quality Mg alloy ingots.
基金supported by the National Natural Scientific Foundation of China(21175112)the Fund of Key Laboratory of Global Change and Marine-Atmospheric Chemistry,SOA,(GCMAC 1204)the Fujian Key Projects of Science and Technology(2011YZ0001-1)
文摘In this work,we reported a simultaneous determination approach for Pb(II),Cd(II)and Zn(II)atμg L 1concentration levels using differential pulse stripping voltammetry on a bismuth film electrode(BiFE).The BiFE could be prepared in situ when the sample solution contained a suitable amount of Bi(NO)3,and its analytical performance was evaluated for the simultaneous determination of Pb(II),Cd(II)and Zn(II)in solutions.The determination limits were found to be 0.19μg L 1for Zn(II),and0.28μg L 1for Pb(II)and Cd(II),with a preconcentration time of 300 s.The BiFE approach was successfully applied to determine Pb(II),Cd(II)and Zn(II)in tea leaf and infusion samples,and the results were in agreement with those obtained using an atomic absorption spectrometry approach.Without Hg usage,the in situ preparation for BiFE supplied a green and acceptability sensitive method for the determination of the heavy metal ions.
基金financially supported by the marine high-tech industry development projects of Fujian Province(No.2015-19)
文摘An electrochemical flow device has been developed for the determination of heavy metal ions(HMI)in water using multiwalled carbon nanotubes(MWCNTs)/Nafion(NA)/Hg electrode,by mean of diff erential pulse anodic stripping voltammetry coupled with sequential injection analysis.The accuracy of the determination was ensured by the great electrical conductivity of MWCNTs and the high adsorption capacity of Hg.NA was used for MWCNTs immobilization for the long-term application of the electrode.The mercury film was cleaned after determination and another one would form during deposition.A lower limit of detection and a wider determination range of Cd^(2+)and Pb^(2+)could be achieved using the automatically analytical device combining with the MWCNTs/NA/Hg-modified electrode.The real-time monitoring of Cd^(2+)and Pb^(2+)in fresh water using this device continued for 10 days.The results indicated that the method was potential for on-site and real-time determination of HMI in water samples.
基金Project supported by the National Natural Science Foundation of China (No. 20377007).
文摘A novel differential pulse anodic stripping voltammetry for the determination of trace amounts of lead, using a biomacromolecule heparin drop-coated modified glassy carbon electrode, has been described. Pb2+ was deposited on the surface of a heparin-modified electrode at -1.0 V (vs. SCE) via forming Pb2+-heparin and subsequent re-duction at the electrode. In the following step, Pb-heparin was oxidized, and voltammograms were recorded by scanning the potential in a positive direction. Conditions were optimized with respect to the pH of the medium, the mass of drop-coated heparin, accumulation potential and accumulation time. The peak current was proportional to the Pb2+ concentration in the range of 2.0×10-9 to 7.0×10-7 mol/L. The detection limit was 3.0×10-10 mol/L. The relative standard deviation was 4.83% for 1.0×10-8 mol / L Pb2+ (n=10). The developed method has been applied to the determination of Pb2+ in water samples with satisfactory results.
文摘The determination of trace element Pb in electrolyte MnSO_4H_2SO_4 was studied with differential pulse po-larography. The trace Pb was originated from new type Pb-Ag-Ca alloy anode being used in preduction processof electrolytic MnO_2 (EMD). The KCl was added as background of electrolyte. The differential pulse polarco-gram obtained for Pb(Ⅱ) is well in peak contour and is easy to determination. The peak potential is -0. 44 V(vs Ag-AgCl potential , experimental valuel). The Pb content may be determined by standard addition methodwhich is simple , reliable and fast. This study presents some foundamental data for Pb-Ag-Ca anode (abbreviated to PAC anede). The consuming rate for PAC anode is evaluated as 4. 82% annually.
文摘The second derivative differential pulse polarography was developed for the quantitative determination of active principles in medicinal herbs (baicalin in Scutellaria baicalensis Georgi, indigo in Baphicacanthus cusia (Nees) Bremek, paeonol in Paeonia suffruticosa Andr and piperine in Piper longum L ) The C O group in baicalin, indigo, paeonol and piperine could be reduced to CH OH in acidic solution at the dropping mercury electrode, and showed very good second derivative differential pulse polarographic peak at 1 550V, 1 300V, 1 630V and 0 860V (vs Ag/AgCl) respectively The linear relationship between concentration of baicalin, indigo, paeonol, piperine and peak height was obtained in the concentration range of 4 5×10 5 ～ 2 7×10 4 mol·L 1 , 3 8×10 5 ～ 4 2×10 4 mol·L 1 , 1 0～6 0×10 4 mol·L 1 and 7 0×10 5 ～2 5×10 4 mol·L 1 and the determination limits were 9 0×10 8 mol·L 1 , 8 4×10 9 mol·L 1 , 9 2×10 9 mol·L 1 and 8 7×10 9 mol·L 1 respectively This method is simple, rapid and sensitive, and the results are accurate
文摘The potassium phosphate buffer as a supporting electrolyte of anticancer drug(5-fluorouracil(5-FU))was the best among solutions of sodium phosphate buffer and Britton Robinson buffer in differential pulse polarography(DPP)at pH=7.0 and T=37℃.The changes of temperature did not effect on inactivity of the supporting electrolyte(potassium phosphate buffer at T=10-50℃),and pH of the solution did not exceed 2%of each 5℃(at pH=7.0,by modified thermostat cell).However,the frequency measurements showed clear effect of temperature on diffusion current(IP/μA)of the chemotherapy compound in the range of 20-50℃and under primary conditions.Then,the polarography measurements of 5-FU drug(at 10μM,pH=7 and T=37℃)gradually led to the optimum conditions:deposition potential=-0.9 V;drop size=9.0 mm^(3);deposition time=15.0 s;equilibration time=5.0 s;pulse amplitude=100 mV;pulse time=7.0 ms;voltage step=6 mV;voltage step time=0.3 s;and sweep rate=20.0 mV/s.The thermal assessment of 5-FU drug(after achievement of the optimum conditions)in a new thermostat vessel at HMDE by DPP showed that the reaction of 5-FU molecules represented pseudo first order reaction,instead of first order;the secondary waves of 5-FU drug may be due to formation of molecular complexes in aqueous solution and the reduction of 5-FU molecules at mercury surface electrode appeared as physisorption,instead of chemisorption.
文摘The determination of trace rhenium(Ⅶ)by differential pulse polarography in the system of H_2SO_4-(NH_2OH)_2·H_2SO_4-TeO_4^(2-) is markedly improved by the addition of Nitron,which is adsorbed on the surface of mercury electrode.The limit of detection is down to 2×10^(-10) M.The adsorptive peak potential is -0.80V(vs.SCE).In the ranges of 5×10^(-10)-10^(-8),1×10^(-8)-10^(-7) and 1× 10^(-7)-10^(-6)M,there are good linear relationships between the peak current increment and the concentration,of which the relative standard deviations are 9.5,6.6,1.8% respectively with the correlation coefficients of linear regression of 0.995—0.999.The results relating to this polarographic wave show that it is an adsorption-catalytic wave.The mechanism of the electrode reaction is dis- cussed.
文摘Even in small concentrations,toxic metals like lead,cadmium,and mercury are dangerous to the environment and human health.Environmental monitoring depends on precisely identifying these heavy metals,particularly cadmium ions(Cd(Ⅱ)).In this study,we present a novel screen-printed carbon electrode(SPCE)modified with single crystallineα-Fe_(2)O_(3)nano-hexagons that functions as a sensor for detecting Cd(Ⅱ).The performance of the fabricated sensor was thoroughly assessed and compared with unmodified SPCE using the voltammetric method.The crystalline structure of the synthesizedα-Fe_(2)O_(3)nano-hexagons was confirmed through XRD,and surface analysis revealed an average diameter and thickness of 86 nm and 9 nm,respectively.Theα-Fe_(2)O_(3)modified SPCE yields a 7-fold enhanced response(at pH 5.0 vs.Ag/AgCl)to Cd(Ⅱ)than bare SPCE.The modified electrode effectively detects Cd(Ⅱ)with a linear response range of up to 333.0μmol/L and a detection limit of 0.65 nmol/L under ideal circumstances.This newly fabricated sensor offers significant potential for environmental monitoring applications by providing outstanding practicality,anti-interference ability,and repeatability for detecting Cd(Ⅱ)in water samples.
文摘The design and implementation of a novel ADC architecture called ring-ADC for digital voltage regulator module controllers are presented. Based on the principle of voltage-controlled oscillators＇ transform from voltage to frequency,the A/D conversion of ring-ADC achieves good linearity and precise calibration against process variations compared with the delay-line ADC. A differential pulse counting discriminator also helps decrease the power consumption of the ring-ADC. It is fabricated with a Chartered 0.35μm CMOS process, and the measurement results of the integral and differential nonlinearity performance are 0.92LSB and 1.2LSB respectively. The maximum gain error measured in ten sample chips is ± 3.85%. With sampling rate of 500kHz and when the voltage regulator module （VRM） works in steady state, the ring-ADC＇s average power consumption is 2.56mW. The ring-ADC is verified to meet the requirements for digital VRM controller application.
