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1.
Yang Wang  Guojun Yao  Peihua Zhu  Xiaoya Hu  Qin Xu 《Talanta》2010,82(4):1500-2527
The analytical performance of lab-on-valve (LOV) system using irreversible biamperometry for the determination of catechol was evaluated. By integrating miniaturized electrochemical flow cell (EFC) designed and processed which is furnished with two identical polarized platinum electrodes, into the LOV unit, the lab-on-valve system combines sampling with analysis, realizing automated on-line analysis for catechol in a closed system. The biamperometric detection system was established to record the relationship between oxidation current and time by coupling the irreversible oxidation of catechol at one pretreated platinum electrode with the irreversible reduction of platinum oxide at the other pretreated platinum electrode. Factors influencing the analytical performance were optimized, including the potential difference (ΔE), buffer solution and pH, and flow variables in the LOV. A linear calibration curve was obtained within the range of 1.0 × 10−6-5.0 × 10−4 mol L−1 of catechol with the detection limit (3σ) of 5.09 × 10−7 mol L−1. The relative standard deviation (R.S.D.) was 2.39% for 11 successive determinations of 1 × 10−5 mol L−1 catechol and the sample throughput was 35 h−1. Moreover, this proposed method was applied to the analysis of catechol in beer sample, which was testified by high-performance liquid chromatography (HPLC).  相似文献   

2.
Li M  Lee SH 《Talanta》2007,74(2):265-270
A simple, rapid flow injection chemiluminescence (FI-CL) method has been developed for selective determination of acenaphthylene (ACY), based on the CL produced in the reaction of tris(2,2′-bipyridine)ruthenium(III) (Ru(bipy)33+) and ACY in an acidic buffer solution. Under the optimum experimental conditions, the calibration curve was linear over the range 5.0 × 10−3 to 4.0 × 10−7 mol L−1 for ACY. The detection limit (S/N = 3) was 2.0 × 10−7 mol L−1 and the relative standard deviation of 10 replicate measurements was 2.3% for 5.0 × 10−5 mol L−1 of ACY. Selectivity of CL reaction of ACY from other 15 polycyclic aromatic hydrocarbons (PAHs) was investigated by flow injection method. The method was applied to determine the ACY content in soil.  相似文献   

3.
A highly sensitive flow-injection (FI) method with chemiluminescence (CL) detection is used for the determination of l-ascorbic acid. The method is based on the CL reaction of Rhodamine B with cerium(IV) in sulfuric acid media. l-Ascorbic acid is suggested to be a catalyst utilized in the energy-transferred excitation process. The proposed procedure allows quantitation of l-ascorbic acid in the range 3.8×10−13 to 1.0×10−10 mol l−1 with a correlation coefficient of 0.9998 (n=5) and relative standard deviation (R.S.D.) of 0.92% (n=11) at 1.0×10−11 mol l−1. The detection limit (3×blank) was 1.0×10−13 mol l−1. The method is successfully used to determine l-ascorbic acid in fresh vegetables. The possible mechanism of the chemiluminescence in the system is discussed.  相似文献   

4.
A novel, simple, sensitive and precise spectrofluorimetric method was developed for measuring the melamine concentration in different milk batch samples. The method was based upon measuring the quenching of the luminescence intensity of the produced yellow colored ruthenium(II) carbonyl complex of the general formula [Ru(CO)2(L)] (where L = anion of tetradentate Schiff base). The Ru(II) complex exhibited characteristic luminescence band in the visible region. The remarkable quenching of the luminescence intensity of [Ru(CO)2(L)] complex by various concentrations of melamine was successfully used as a chemosensor for the assessment of melamine in different milk samples at λex = 400 nm and pH 7.4 in DMSO with a linear dynamic range 1.0 × 10−6 to 3.0 × 10−9 mol L−1 and lower detection limit (LOD) and quantification detection limit (QOD) of 3.3 × 10−10 and 1.0 × 10−9 mol L−1, respectively.  相似文献   

5.
A novel voltammetric sensor for O,O-dimethyl-(2,4-dichlorophenoxyacetoxyl)(3′-nitrophenyl)methinephosphonate (Phi-NO2) based on molecularly imprinted polymer (MIP) film electrode is constructed by using sol-gel technology. The sensor responds linearly to Phi-NO2 over the concentration range of 2.0 × 10−5 to 1.0 × 10−8 mol L−1 and the detection limit is 1.0 × 10−9 mol L−1 (S/N = 3). This sensor provides an efficient way for eliminating interferences from coexisting substances in the solution. The high sensitivity, selectivity and stability of the sensor demonstrates its practical application for a simple and rapid determination of Phi-NO2 in cabbage samples.  相似文献   

6.
This work reports a sequential-injection analysis (SIA) method for the enzymatic assay of glucose with soluble glucose oxidase (GOD) and on-line sample dilution with chemiluminescence (CL) detection. A zone of sample was aspirated in the holding coil of the SIA manifold and, if necessary, was diluted on-line by means of an auxiliary dilution conduit. Then, a zone of GOD was aspirated adjacent to the sample zone and a stopped-flow period was applied to allow the enzymatic reaction to proceed with production of hydrogen peroxide. Then, zones of a catalyst (Co(II) solution) and alkaline luminol were aspirated into the holding coil. Finally, the flow was reversed and the stacked zones were sent to a flow-cell located in front of a photomultiplier tube (PMT) that monitored the CL intensity. The linear dynamic range was 1 × 10−5-1 × 10−3 mol L−1 glucose, the coefficient of variation at 8 × 10−5 mol L−1 of glucose was sr = 3.1% (n = 8), the limit of detection at the 3σ level was cL = 1 × 10−6 mol L−1 and the sampling frequency was 28 h−1. With on-line dilution by a factor of 1/200, the linear range could be extended up to 0.2 mol L−1 glucose. The advantages of the proposed method are the simple manifold and instrumentation used, the scope for automated on-line dilution, the low consumption of sample and reagents and the elimination of enzyme immobilisation procedures. The method was applied to the analysis of commercial drinks and honey with percent relative errors in glucose determination in the range 100 ± 6.1%.  相似文献   

7.
A carboxyl functionalized graphene oxide (GO-COOH) and electropolymerized ploy-l-lysine (PLLy) modified glassy carbon electrode (GCE) was fabricated and used for the construction of an electrochemical deoxyribonucleic acid (DNA) biosensor. The NH2 modified probe ssDNA sequences were immobilized on the surface of GO-COOH/PLLy/GCE by covalent linking with the formation of amide bonds, which was stable and furthur hybridized with the target ssDNA sequence. Differential pulse voltammetry (DPV) was used to monitor the hybridization events with methylene blue as electrochemical indicator, which gave a sensitive reduction peak at −0.287 V (vs. SCE). Under the optimal conditions the reduction peak current was proportional to the concentration of tlh gene sequence in the range from 1.0 × 10−12 to 1.0 × 10−6 mol L−1 with a detection limit as 1.69 × 10−13 mol L−1 (3σ). The polymerase chain reaction products of tlh gene from oyster samples were detected with satisfactory results, indicating the potential application of this electrochemical DNA sensor.  相似文献   

8.
Ayman A. Abdel Aziz 《Talanta》2010,80(3):1356-1363
A highly selective membrane electrodes based on a two newly synthesized nickel (II) Schiff bases, [NiL1] and [NiL2] where L1 and L2 are N,N/bis(salicylaldehyde)4,5-dimethyl-1,2-phenylenediamine (H2L1) and N,N/bis(salicylaldehyde)4,5-dichloro-1,2-phenylenediamine (H2L2) were used as a neutral carrier ionophores for static and hydrodynamic potentiometric mode of operations for the determination of periodate. Under static mode of operation, the sensors displayed a near-Nernstian slope of −66.1 ± 0.8 and −59.9 ± 1.1 mV decade−1 of activity and detection limits to 5.2 × 10−6 and 7.3 × 10−6 mol L−1 for the sensors based on [NiL1] and [NiL2], respectively. Under hydrodynamic mode of operation (FIA), the slope of the calibration plot, limit of detection, and working linear range were −71.1 mVdecade−1 of activity, 7.3 × 10−6 and 1.0 × 10−5 to 1.0 × 10−3 mol L−1, respectively. The response time of the sensors in whole concentration ranges was very short (<10 s). The response of the sensors was independent on the pH range of 3-8. A tubular version was further developed and coupled to a flow injection system for ascorbic acid (AA) determination in beverages and pharmaceutical preparations. This approach was achieved by selecting a 50-cm reactor and an overall flow of 3 mL min−1, and injecting volume 100 μL of AA standards in a 1.0 × 10−4 mol L−1 IO4 solution. Under these conditions, a linearity range of 2-13 μg mL−1, with a slope of 4.97 mV (mg/L)−1 (r2 = 0.9995), detection limit 0.9 mg L−1 and a reproducibility of ±1.1 mV (n = 5) was recorded. This simple and inexpensive flow injection analysis manifold, with a good potentiometric detector, enabled the analysis of ∼50 samples h−1 without requiring pretreatment procedures. An average recovery of 98.8% and a mean standard deviation of 1.3% were obtained.  相似文献   

9.
Wang X  Lv Y  Hou X 《Talanta》2011,84(2):382-386
The interaction between mercaptoacetic acid (MA)-capped CdTe QDs, MA-capped CdTe/ZnS QDs or glutathione (GSH)-capped CdTe QDs with As(III) was studied using fluorescence spectrometry. As (III) has a high-affinity to reduced-GSH to form As(SG)3, and the emission of the GSH-capped CdTe QDs (λem. = 612 nm) is quenched effectively. Thus, a novel fluorescence spectrometric method was developed for As (III) determination by using GSH-CdTe QDs. Under optimal conditions, the quenched fluorescence intensity (F0/F) increased linearly with the concentration of As (III) ranging from 5.0 × 10−6 to 25 × 10−5 mol L−1. The limit of detection (3σ) for As (III) was found to be 2 × 10−8 mol L−1. This method is potentially useful in visual detection of As (III) under irradiation of the ultraviolet light.  相似文献   

10.
Xiang Y  Mei L  Li N  Tong A 《Analytica chimica acta》2007,581(1):132-136
A new fluorogenic method for the selective and sensitive determination of chromium(VI) in acidic water using rhodamine B hydrazide was developed. This method was based on the oxidation of non-fluorescent rhodamine B hydrazide by potassium dichromate in acidic aqueous conditions to give rhodamine B, which was highly fluorescent, as a product. With the optimum condition described, the fluorescence enhancement at 585 nm was linearly related to the concentration of chromium(VI) in the range of 5.0 × 10−8 to 2.0 × 10−6 mol L−1 (2.60-104 ng mL−1) with a correlation coefficient of R2 = 0.9993 (n = 18) and a detection limit of 5.5 × 10−9 mol L−1 (0.29 ng mL−1). The R.S.D. was 2.2% (n = 5). The proposed method was also applied to the determination of chromium(VI) in drinking water, river water and synthetic samples.  相似文献   

11.
A simple, rapid and sensitive synchronous fluorescence method is put forward for the determination of enrofloxacin (ENRO) in the pharmaceutical formulation and its residue in milk based on the yttrium (III)-perturbed luminescence. When Y3+ is added into the ENRO solution, the fluorescence of ENRO is significantly enhanced. The synchronous fluorescence technology is employed in the method to determine trace amount of ENRO residue in milks. The synchronous fluorescence intensity of the system is measured in a 1-cm quartz cell with excitation wavelength of 328 nm, Δλ = 80 nm. A good linear relationship between the fluorescence intensity and the ENRO concentration is obtained in the range of 1.0 × 10−9 to 2.0 × 10−6 mol L−1 (r2 = 0.9992). The limit of detection (LOD) of this method attains as low as 3.0 × 10−10 mol L−1 (S/N = 3). The selectivity of this method is also very good. Common metal ions, rare-earth ions and some pharmaceuticals, which are usually used together with ENRO, do not interfere with the determination of ENRO under the actual conditions. The proposed method can be applied to determine ENRO residue in milks, and limit of quantification (LOQ) determined in the spiked milk is estimated to be 2.8 × 10−8 mol L−1 (10 μg L−1). Moreover, this method can be used as a rapid screening for judging whether the ENRO residues in milks exceed Minimal Risk Levels (MRLs) or not. In addition, the mechanism of the fluorescence enhancement is also discussed in detail.  相似文献   

12.
Ding SN  Xu JJ  Zhang WJ  Chen HY 《Talanta》2006,70(3):572-577
Tris(2,2′-bipyridyl)ruthenium(II) (Ru(bpy)32+)-Zirconia-Nafion composite modified glassy carbon disk electrode as a solid-state electrochemiluminescence (ECL) detector is successfully applied to an electrophoretic microchip system with a wall-jet configuration. Pharmaceuticals such as tramadol, lidocaine and ofloxacin were selected to characterize the performance of this microchip capillary electrophoresis (CE)-ECL detection system. Voltammetric and ECL behaviors of immobilized Ru(bpy)32+ were investigated in lidocaine system. Influences of the separation electric field to cyclic voltammograms (CVs) of the immobilized Ru(bpy)32+ were also investigated. Tramadol, lidocaine and ofloxacin can be baseline separated without any additives. The detection limits (S/N = 3) were 2.5 × 10−5 mol L−1 for tramadol, 5.0 × 10−6 mol L−1 for lidocaine, 1.0 × 10−5 mol L−1 for ofloxacin under the sample injection of picoliters, and the linear ranges were from 5.0 × 10−5 to 2.5 × 10−3 mol L−1 for tramadol, 1.0 × 10−5 to 1.0 × 10−3 mol L−1 for lidocaine, and 1.0 × 10−5 to 2.5 × 10−3 mol L−1 for ofloxacin, respectively.  相似文献   

13.
The effect of detection chip geometry on chemiluminescence (CL) signal intensity of tris(1,10-phenanthroline)-ruthenium(II) peroxydisulphate system for analysis of chlorpheniramine maleate (CPM) in pharmaceutical formulations was investigated. It was observed that the design of the detection chip is very crucial and can play an important role in enhancing the CL signal intensity in this system. The CL signal intensity was enhanced 250% when a teardrop micromixer chip was used, compared to the commonly used serpentine chip geometry. The study was conducted using a multi-chip device. In this device, chip 1 was used to prepare and pump the reagent mixture, whereas chip 3 was used for pumping the sample. The two chips were connected to the teardrop chip (2) via silica capillary where detection took place. Non-linear regression curve fitting of the calibration data revealed that the calibration curves are best described by third order polynomial equation with excellent correlation coefficients (R2 = 0.9998) for the concentration range 7.69 × 10−8 to 5.12 × 10−5 mol L−1. A linear response is also observed over the range 7.69 × 10−8 to 1.28 × 10−5 mol L−1 (R2 = 0.9996) and the detection limit was found to be 5.49 × 10−8 mol L−1. The device was successfully used for the analysis of CPM in tablets and a multi-component cough syrup. Results were reproducible with relative standard deviation (RSD) of 0.6-1.1%.  相似文献   

14.
Zhang J  Zhang Z  Xiang Y  Dai Y  Harrington Pde B 《Talanta》2011,84(5):1401-1409
A sequential injection analysis (SIA) spectrophotometric method for determining tetracycline (TC), chlortetracycline (CTC) and oxytetracycline (OTC) in different sample matrices were described. The method was based on the reaction between tetracyclines and yttrium (III) in weak basic micellar medium, yielding the light yellow complexes, which were monitored at 390, 392 and 395 nm, respectively. A cationic surfactant, cetyltrimethylammonium bromide (CTAB) was used to obtain the micellar system. The linear ranges of calibration graphs were between 1.0 × 10−5 and 4 × 10−4 mol L−1, respectively. The molar absorptivities were 5.24 × 105, 4.98 × 104 and 4.78 × 104 L mol−1 cm−1. The detection limits (3σ) were between 4.9 × 10−6 and 7.8 × 10−6 mol L−1 whereas the limit of quantitations (10σ) were between 1.63 × 10−5 and 2.60 × 10−5 mol L−1 the interday and intraday precisions within a weak revealed as the relative standard deviations (R.S.D., n = 11) were less than 4%. The method was rapid with a sampling rate of over 60 samples h−1 for the three drugs. The proposed method has been satisfactorily applied for the determination of tetracycline and its derivatives in pharmaceutical preparations together with their residues in milk and honey samples collected in Chiang Mai Province. The accuracy was found to be high as the Student's t-values were found to be less than the theoretical ones. The results were compared favorably with those obtained by the conventional spectrophotometric method.  相似文献   

15.
Mehretie S  Admassie S  Hunde T  Tessema M  Solomon T 《Talanta》2011,85(3):1376-1382
A sensitive and selective method was developed for the determination of N-acetyl-p-aminophenol (APAP) and p-aminophenol (PAP) using poly(3,4-ethylenedioxythiophene) (PEDOT)-modified glassy carbon electrode (GCE). Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical reaction of APAP and PAP at the modified electrode. Both APAP and PAP showed quasireversible redox reactions with formal potentials of 367 mV and 101 mV (vs. Ag/AgCl), respectively, in phosphate buffer solution of pH 7.0. The significant peak potential difference (266 mV) between APAP and PAP enabled the simultaneous determination both species based on differential pulse voltammetry. The voltammetric responses gave linear ranges of 1.0 × 10−6-1.0 × 10−4 mol L−1 and 4.0 × 10−6-3.2 × 10−4 mol L−1, with detection limits of 4.0 × 10−7 mol L−1 and 1.2 × 10−6 mol L−1 for APAP and PAP, respectively. The method was successfully applied for the determination of APAP and PAP in pharmaceutical formulations and biological samples.  相似文献   

16.
Zhang Y  Zheng J 《Talanta》2008,77(1):325-330
An ionic liquid modified carbon paste electrode (IL/CPE) had been fabricated by using hydrophilic ionic liquid 1-amyl-3-methylimidazolium bromide ([AMIM]Br) as a modifier. The IL/CPE was characterized by scanning electron microscope and voltammetry. Electrochemical behavior of rutin at the IL/CPE had been investigated in pH 3.29 Britton-Robinson (B-R) buffer solution by cyclic voltammetry (CV) and square wave voltammetry (SWV). The experimental results suggested that the modified electrode exhibited an electrocatalytic activity toward the redox of rutin. The electron transfer coefficient (α) and the standard rate constant (ks) of rutin at the modified electrode were calculated. Under the selected conditions, the reduction peak current was linearly dependent on the concentration of rutin in the range of 4.0 × 10−8 to 1.0 × 10−5 mol L−1 (r = 0.9998), with a detection limit of 1.0 × 10−8 mol L−1 (S/N = 3). The relative standard deviation (R.S.D.) for six times successful determination of 8.0 × 10−7 mol L−1 rutin was 1.2%. The proposed method was applied to determine rutin in tablet and urine sample. In addition, the IL/CPE exhibited a distinct advantage of simple preparation, surface renewal, good reproducibility and good stability.  相似文献   

17.
The paper presents the first report on fabrication and application of a user friendly and mercury free electrochemical sensor, with the renewable bismuth bulk annular band working electrode (RBiABE), in stripping voltammetry (SV). The sensor body is partly filled with the internal electrolyte solution, in which the RBiABE is cleaned and activated before each measurement. Time of the RBiABE contact with the sample solution is precisely controlled. The usefulness of this sensor was tested by Ni(II) and Co(II) traces determination by means of differential pulse adsorptive stripping voltammetry (DP AdSV), after complexation with dimethylglyoxime (DMG) in ammonia buffer (pH 8.2). The experimental variables (composition of the supporting electrolyte, pre-concentration potential and time, potential of the RBiABE activation, and DP parameters), as well as possible interferences, were investigated. The linear calibration graphs for Ni(II) and Co(II), determined individually and together, in the range from 1 × 10−8 to 70 × 10−8 mol L−1 and from 1 × 10−9 to 70 × 10−9 mol L−1 respectively, were obtained. The calculated limit of detection (LOD), for 30 s of the accumulation time, was 3 × 10−9 mol L−1 for Ni(II) in case of a single element’s analysis, whereas the LOD was 5 × 10−9 mol L−1 for Ni(II) and 3 × 10−10 mol L−1 for Co(II), when both metal ions were measured together. The repeatability of the Ni(II) and Co(II) adsorptive stripping voltammetric signals obtained at the RBiABE were equal to 5.4% and 2.5%, respectively (n = 5). Finally, the proposed method was validated by determining Ni(II) and Co(II) in the certified reference waters (SPS-SW1 and SPS-SW2) with satisfactory results.  相似文献   

18.
Su Y  Wang J  Chen G 《Talanta》2005,65(2):531-536
Epinephrine was found to be able to strongly enhance the electrochemiluminescence (ECL) of lucigenin system by using the anodic potential sweep. Based on which, a novel ECL method for the determination of epinephrine was developed. Under the optimum condition, the enhanced ECL intensity was linear with the epinephrine concentration in the range of 4.0 × 10−8 to 2.0 × 10−7 mol L−1. The detection limit (defined as S/N = 3) was 2.4 × 10−8 mol L−1, and the relative standard deviation was 2.7% for 1.0 × 10−7 mol L−1 epinephrine (n = 11). The method was successfully applied to the determination of epinephrine in pharmaceutical samples with satisfactory results. In addition, the possible mechanism for the lucigenin ECL system in the presence of epinephrine has also been discussed.  相似文献   

19.
A new palladium nanoparticle functionalized multi-wall carbon nanotubes (nano-Pd/CNTs) modified pyrolytic graphite electrode (PGE) has been fabricated for electrochemical sensing of calcium dobesilate (CD) in pharmaceutical capsules. The nano-Pd/CNTs were characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The nano-Pd/CNTs composite showed a strong electrocatalytic property for CD. The anodic peak current is 6-fold than that obtained in bare PGE and the oxidation potential has an obvious shift to negative. The anodic peak current is proportional to the concentration of CD in the range of 1.0 × 10−7 to 7.0 × 10−4 mol L−1, with a linear relative coefficient r = 0.999 and a detection limit 4.0 × 10−8 mol L−1 (S/N = 3). This kind of electrode shows good stability, sensitivity, reproducibility, large linear range and low detection limit towards electrochemical determination of CD. The proposed method provides a selective and sensitive electrochemical sensor of calcium dobesilate.  相似文献   

20.
A plasticized poly (vinyl chloride) membrane electrode based on 1,3-bis(2-cyanobenzene)triazene (CBT) for highly selective determination of platinum(II) (in PtCl42− form) is developed. The electrode showed a good Nernstian response (29.8 ± 0.3 mV decade−1) over a wide concentration range (1.0 × 10−6 to 1.0 × 10−2 mol L−1). The limit of detection was 5.0 × 10−7 mol L−1. The electrode has a response time of about 40 s, and it can be used for at least 1 month without observing any considerable deviation from Nernstian response. The proposed electrode revealed an excellent selectivity toward platinum(II) ion over a wide variety of alkali, alkaline earth, transition, and heavy metal ions, and it could be used in the pH range of 3.2-5.1. The practical utility of the electrode has been demonstrated by its use in determination of platinum ion in, alloy, tap, mineral and river water samples.  相似文献   

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