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1.
A supported liquid membrane system has been developed for the extraction of vanillin from food samples. A porous PTFE membrane is impregnated with an organic solvent, which forms a barrier between two aqueous phases. The analyte is extracted from a donor phase into the hydrophobic membrane and then back extracted into a second aqueous solution, the acceptor. The determination (100–1400 μg ml−1 vanillin) was performed using a PVC-graphite composite electrode versus Ag/AgCl/3MKCl at +0.850 V placed in a wall-jet flow cell as amperometric detector. The solid sample is directly placed in the membrane unit without any treatment, and the analyte was extracted from the sample, passes through the membrane and conduced to the flow cell by the acceptor stream. The limit of detection (3σ) was 44 μg ml−1. The method was applied to the determination of vanillin (9–606 μg g−1) in food samples.  相似文献   

2.
Ruengsitagoon W 《Talanta》2008,74(5):1236-1241
A simple reversed flow injection colourimetric procedure for determining iron(III) was proposed. It is based on the reaction between iron(III) with chlortetracycline, resulting in an intense yellow complex with a suitable absorption at 435 nm. A 200 μl chlortetracycline reagent solution was injected into the phosphate buffer stream (flow rate 2.0 ml min−1) which was then merged with iron(III) standard or sample in dilute nitric acid stream (flow rate 1.5 ml min−1). Optimum conditions for determining iron(III) were investigated by univariate method. Under the optimum conditions, a linear calibration graph was obtained over the range 0.5–20.0 μg ml−1. The detection limit (3σ) and the quantification limit (10σ) were 0.10 and 0.82 μg ml−1, respectively. The relatives standard deviation of the proposed method calculated from 12 replicate injections of 2.0 and 10.0 μg ml−1 iron(III) were 0.43 and 0.59%, respectively. The sample throughput was 60 h−1. The proposed method has been satisfactorily applied to the determination of iron(III) in natural waters.  相似文献   

3.
Wang J  Zhang C  Wang H  Yang F  Zhang X 《Talanta》2001,54(6):146-1193
A simple, fast chemiluminescence (CL) flow-injection method based on the reaction of luminol with H2O2 in the presence of a cationic surfactant (cyltrimethylammonium bromide, CTMAB) has been described for the direct determination of dichlorvos pesticide (DDVP). Under the optimal conditions, the CL intensity was linear to the DDVP concentration in the range of 0.02–3.1 μg ml−1 (r=0.9998, n=10). The relative standard deviation was 3.4% at 0.35 μg ml−1 (n=10), with a detection limit (3σ) of 0.008 μg ml−1 DDVP. The possible reaction mechanism was also discussed. This method has been successfully applied to the determination of trace DDVP residue in vegetable sample and results have been compared with that of the UV method.  相似文献   

4.
A continuous flow system for the determination of lead in home made spirituous beverages was developed. The determination was based on the formation of a neutral chelate of the element with ammonium pyrrolidine dithiocarbamate, its adsorption onto a minicolumn packed with sodium faujasite type Y synthetic zeolite, followed by elution with methyl isobutyl ketone and determination by flame atomic absorption spectrometry. Ethanol and copper interfere strongly in the determination and therefore, must be separated prior to the analysis. Copper is removed by precipitation with rubeanic acid, while ethanol is eliminated by rotaevaporation. Sample solutions containing Pb2+ in the concentration range from 5 to 120 μg l−1 at pH 2.5 could be analyzed, by using a preconcentration time of 3 min. Preconcentration factors from 80 to 140 were achieved for a sample volume of 6 ml and the detection limit varied from 1.4 to 3.5 μg l−1, depending on the matrix composition. The relative standard deviations for 60 μg l−1 Pb was 3.2% (n = 10) and the recovery of spikes (20, 40, 60 and 80 μg l−1) added to the samples was estimated within 92–105% range, suggesting that lead can be quantitatively determined in such samples. Determining lead in several samples by an alternative technique further checked the accuracy. Finally, the concentrations of Pb2+ determined in 28 samples of Venezuelan spirituous beverages were in 12.6–370.0 μg l−1 range, depending on the fermenting material based on different mixtures of agave, raw sugar cane and white sugar.  相似文献   

5.
A sensitive method for the post-column reaction detection of organophosphorus pesticides is described. The method relies on photolysis of the organocompounds by irradiation with a low-pressure mercury lamp (main spectral line, 254 nm) in the presence of peroxydisulfate. The resultant orthophosphate was reacted with molybdate to form molybdophosphoric acid, which subsequently reacted with thiamine to generate thiochrome. Finally, the fluorescence intensity of thiochrome was measured at 440 nm with excitation at 375 nm. Factors affecting the rate of these reactions were optimized so that its contribution to the total band-broadening was negligible.

This detection system was used for the determination of phosphate, acephate and methamidophos, which were separated on an ODS column by isocratic reversed phase chromatography with acetonitrile–water as the mobile phase. A linear relationship between analyte concentration and peak area was obtained within the range 0.016–7.0 μg ml−1 with correlation coefficients greater than 0.9995 and detection limits between 4 and 12 ng ml−1. Intra- and inter-day precision values of about 1.2% R.S.D. (n = 10) and 2.1% R.S.D. (n = 30), respectively, were obtained.

Pesticide residues below ng ml−1 levels could be determined in environmental waters when a preconcentration device was coupled on-line with the HPLC system. Detection limits as low as 0.01 ng ml−1 were achieved for only 250 ml of sample. In the analyses of vegetables and grains, the detection limit was about 1 μg kg−1.  相似文献   


6.
A sequential injection analysis (SIA) spectrophotometric method for the determination of trace amounts of zinc(II) with 1-(2-pyridylazo)-2-naphthol (PAN) is described. The method is based on the measurement of absorbance of the zinc(II)–PAN chelate solubilized with a non-ionic surfactant, Triton X-100, no extraction procedure is required in the proposed method, yielding a pink colored complex at pH 9.5 with absorption maximum at 553 nm. The SIA parameters that affect the signal response have been optimized in order to get the better sensitivity and minimum reagent consumption. A linear relationship between the relative peak height and concentration was obtained in the concentration range of 0.1–1.0 μg ml−1. The limit of detection (LOD, defined as 3σ) and limit of quantification (LOQ, defined as 10σ) were 0.02 and 0.06 μg ml−1, respectively. The sample throughput about 40 samples/h was obtained. The repeatability were 1.32 and 1.24% (n = 10) for 0.1 and 0.5 μg ml−1, respectively. The proposed method was successfully applied to the assay of zinc(II) in three samples of multivitamin tablets. The results were found to be in good agreement with those obtained by flame atomic absorption spectrophotometric method and with the claimed values by the manufactures. The t-test showed no significant difference at 95% confidence level.  相似文献   

7.
Zhou X  Xing D  Zhu D  Tang Y  Jia L 《Talanta》2008,75(5):1300-1306
Enrofloxacin (ENR) is a fluoroquinolone developed exclusively for the use in veterinary practice for the treatment of respiratory and gastrointestinal infections, and ciprofloxacin (CIP) is its main active metabolite. Their contents are regulated by the EU Council Regulation no. 2377/90 in animal edible tissues. We developed a sensitive and rapid method for the determination of ENR and CIP by capillary electrophoresis (CE) with electrochemiluminescence (ECL) detection. The method is based on the detection of aliphatic tertiary or secondary amino moieties in ENR and CIP with end-column tris(2,2-bipyridyl)ruthenium(II) electrochemiluminescence. Parameters that affect separation and detection were optimized. Under the optimized conditions, the calibration functions were linear in the range of 0.03–1 μg ml−1 for ENR and 0.05–1.2 μg ml−1 for CIP. The detection limits of ENR and CIR were 10 ng ml−1 and 15 ng ml−1, respectively, based on the signal-to-noise ratio of 3. The relative standard derivations of the peak height and the migration time for ENR and CIP were less than 4.13%. The developed method was successfully applied to determine ENR and CIP in milk with a solid-phase extraction procedure.  相似文献   

8.
An atomic absorption spectrophotometric method for the determination of trace copper after adsorption of its 1-nitroso-2-naphthol-3,6-disulfonic acid chelate on Ambersorb 572 has been developed. This chelate is adsorbed on the adsorbent in the pH range 1–8. The copper chelate is eluted with 5 ml of 0.1 mol l−1 potassium cyanide and determined by flame atomic absorption spectrometry (FAAS). The selectivity of the proposed procedure was also evaluated. Results show that iron(III), zinc(II), manganese(II) and cobalt(II) at the 50 μg l−1 level and sodium(I), potassium(I), magnesium(II), calcium(II) and aluminium(III) at the 1000 μg l−1 level did not interfere. A high enrichment factor, 200, was obtained. The detection limit (3σ) of copper was 0.34 μg l−1. The precision of the method, evaluated by seven replicate analyses of solutions containing 5 μg of copper was satisfactory and the relative standard deviation was 1.7%. The adsorption of copper onto Ambersorb 572 can formally be described by a Langmuir equation with a maximum adsorption capacity of 14.3 mg g−1 and a binding constant of 0.00444 l mg−1. The accuracy of the method is confirmed by analysing tomatoes leaves (NIST 1573a) and lead base alloy (NBS 53e). The results demonstrated good agreement with the certified values. This procedure was applied to the determination of copper in waters (tap, river and thermal waters), aluminium foil and tea samples.  相似文献   

9.
For the first time a new, sensitive, and simple bead injection spectroscopy–flow injection analysis (BIS–FIA) system with spectrofluorimetric detection is described for the sequential determination of two metals. The sensor is based on the alternate use of two carriers and a commercially available flow cell (Hellma 176-QS). The flow cell is filled by injecting in the flow system 500 μl of a homogeneous bead suspension of an appropriate solid support (Sephadex QAE A-25) previously loaded with the fluorogenic reagent morin (2′,3,4′,5,7-pentahydroxyflavone). A sequential reaction of Al(III) and Be(II) with morin (immobilized on beads) to form their fluorescent complexes is performed on the bead sensing support and their respective fluorescence emission monitored, after doing two successive injections from the mixture solution. Firstly, Al(III) could be determined in the sample using 0.5 M NaCl/HCl, pH 6 as carrier. Then, the carrier solution was changed (0.3 M NaCl/NaOH, pH 12) making possible the elution of Al(III) and the restoration of the baseline, then allowing the reaction of Be(II). At the end of the analysis, beads are automatically discarded from the flow cell, by reversing the flow, and transported out of the system. The analytical signals are measured at an excitation wavelength of 440 nm and an emission wavelength of 520 nm. Using a sample volume of 600 μl, the analytical signal showed a very good linearity in the range 0.1–8 ng ml−1 and 0.1–1 μg ml−1 with detection limits of 0.024 ng ml−1 and 0.010 μg ml−1 for Be(II) and Al(III), respectively. R.S.D.s (%) lower than 5% were obtained for both analytes and the selectivity was improved using EDTA as masking reagent. The sensor was satisfactorily applied to the determination of these metals in waters and simulated alloy samples.  相似文献   

10.
Pulsed amperometric detection of furan compounds in transformer oil   总被引:1,自引:0,他引:1  
The failure of high voltage transformers can result in significant cost and supply implications to both power supplier and consumer alike and in extreme cases may result in explosion, serious injury or death. Transformer failure can be predicted by measuring furanics present in the oil, produced by the thermolytic breakdown of cellulosidic insulators. Failing units can have furanic levels of up to 10 μg ml−1. The use of pulsed amperometric detection (PAD) to measure furanics in transformer oils in real time is reported here. Oils were examined by pre-extraction or direct suspension in aqueous measurement solution or by solubilisation and direct PAD measurement in organic solvents. Linear relationships between PAD response and furanic concentration was found for 2-furaldehyde and furfuryl alcohol (F-OH) across the range of 0–10 μg ml−1, with PAD proving most sensitive to the latter compound. PAD was performed directly in the organic phase in t-butanol with 0.1 M tetramethyl ammonium hydroxide, with aged oils containing >2 μg ml−1 of 2-furaldehyde yielding data within close agreement (<9%) of a standard chromatographic method. The simplicity and rapidity of this method offers the power transmission industry a means of monitoring furanic levels in transformers in real time, thereby reducing the risk of uncontrolled transformer failure.  相似文献   

11.
Yun Fei Long  Cheng Zhi Huang   《Talanta》2007,71(5):1939-1943
The interaction of Amido black 10B (AB) with DNA in basic medium was studied in the presence of cetyltrimethylammonium bromide (CTMAB) based on the measurements of resonance light scattering (RLS), UV–vis, CD spectra, and RLS imaging. The interaction has been proved to give a ternary complex of CTMAB–DNA–AB in Britton–Robinson buffer of pH 11.55, which exhibits strong negative Cotton effect at 233.3 nm and 642.8 nm, and strong RLS signals characterized at 469 nm. Experiments showed that the enhanced RLS intensities (ΔIRLS) against the mixture of AB and CTMAB are proportional to the concentration of fish sperm DNA (fsDNA) and calf thymus DNA (ctDNA), respectively over the range of 0.03–1.0 and 0.05–1.5 μg ml−1, with the limits of determination (3σ) of 7.3 ng ml−1 for fsDNA and 7.0 ng ml−1 for ctDNA.  相似文献   

12.
An analytical method for analysing acrylamide in coffee was validated. The analysis of prepared coffee includes a comprehensive clean-up using multimode solid-phase extraction (SPE) by automatic SPE equipment and detection by liquid chromatography tandem mass spectrometry using electrospray in the positive mode. The recoveries of acrylamide in ready-to-drink coffee spiked with 5 and 10 μg l−1 were 96±14% and 100±8%, respectively. Within laboratory reproducibility for the same spiking levels were 14% and 9%, respectively. Coffee samples (n = 25) prepared twice by coffee machines and twice by a French Press Cafetière coffee maker contained 8±3 μg l−1 and 9±3 μg l−1 acrylamide. Five ready-to-drink instant coffee prepared twice contained 8±2 μg l−1. Hence, the results do not show significant differences in the acrylamide contents in ready-to-drink coffee prepared by coffee machine, French Press or from instant coffee. Medium roasted coffee contained more acrylamide (10 μg l−1) than dark roasted coffee (5 μg l−1). Males aged 35–45 years, drinking on average 1.1 l coffee per day are exposed to the highest doses of acrylamide from coffee. The dietary intake of acrylamide from coffee comprises, on an average, 10 μg day−1 for males and 9 μg day−1 for females aged 35–45 years. Probabilistic modelling of the exposure of Danish consumers (all adults) to acrylamide from coffee shows a mean exposure of 6.5 μg day−1 and a 95 percentile of 18 μg day−1.  相似文献   

13.
Polystyrene–divinylbenzene (8%) has been functionalised by coupling it through an ---N=N--- group with 6-mercaptopurine. The resulting chelating resin has been characterised by using elemental analysis, thermogravimetric analysis and infrared spectra. The resin is highly selective for Hg(II) and Ag(I) and has been used for preconcentrating Hg(II) and Ag(I) prior to their determination by atomic absorption spectrometry. The maximum sorption capacity for Hg(II) and Ag(I) was found to be 1.74 and 0.52 mmol g−1, respectively, over the pH range 5.5–6.0. The calibration range for Hg(II) was linear up to 10 ng ml−1 with a 3σ detection limit of 0.02 ng ml−1; the calibration range for Ag(I) was linear up to 5 μg ml−1 with a detection limit of 29 ng ml−1. The recoveries of the metals were found to be 99.7±3.8 and 101.3±4.1% at the 95% confidence level for both Hg(II) and Ag(I). In column operation, it has been observed that Hg(II) and Ag(I) in trace quantities can be selectively separated from geological, medicinal and environmental samples.  相似文献   

14.
A simple procedure was developed for the direct determination of As(III) and As(V) in water samples by flow injection hydride generation atomic absorption spectrometry (FI–HG–AAS), without pre-reduction of As(V). The flow injection system was operated in the merging zones configuration, where sample and NaBH4 are simultaneously injected into two carrier streams, HCl and H2O, respectively. Sample and reagent injected volumes were of 250 μl and flow rate of 3.6 ml min−1 for hydrochloric acid and de-ionised water. The NaBH4 concentration was maintained at 0.1% (w/v), it would be possible to perform arsine selective generation from As(III) and on-line arsine generation with 3.0% (w/v) NaBH4 to obtain total arsenic concentration. As(V) was calculated as the difference between total As and As(III). Both procedures were tolerant to potential interference. So, interference such as Fe(III), Cu(II), Ni(II), Sb(III), Sn(II) and Se(IV) could, at an As(III) level of 0.1 mg l−1, be tolerated at a weight excess of 5000, 5000, 500, 100, 10 and 5 times, respectively. With the proposed procedure, detection limits of 0.3 ng ml−1 for As(III) and 0.5 ng ml−1 for As(V) were achieved. The relative standard deviations were of 2.3% for 0.1 mg l−1 As(III) and 2.0% for 0.1 mg l−1 As(V). A sampling rate of about 120 determinations per hour was achieved, requiring 30 ml of NaBH4 and waste generation in order of 450 ml. The method was shown to be satisfactory for determination of traces arsenic in water samples. The assay of a certified drinking water sample was 81.7±1.7 μg l−1 (certified value 80.0±0.5 μg l−1).  相似文献   

15.
Cui X  Fang G  Jiang L  Wang S 《Analytica chimica acta》2007,590(2):2139-259
A simple and sensitive kinetic-spectrophotometric method was developed for the determination of ultra trace amount of formaldehyde in food samples. The method was based on the oxidation of rhodamine B (RhB) by potassium bromate in sulfuric acid medium (formaldehyde as catalyst). The reaction was monitored by measuring the decrease in absorbance of the dye at 515 nm after 6 min. The developed method allowed the determination of formaldehyde in the range of 10–100 μg L−1 with good precision, accuracy and the detection limit was down to 2.90 μg L−1. The relative standard deviations for the determination of 10 and 60 μg L−1 of formaldehyde were 3.0% and 1.9% (n = 10), respectively. The method was found to be sensitive, selective and was applied to the determination of formaldehyde in foods with satisfactory results.  相似文献   

16.
Soylak M  Tuzen M  Mendil D  Turkekul I 《Talanta》2006,70(5):1129-1135
A solid phase extraction procedure based on biosorption of copper(II), lead(II), zinc(II), iron(III), nickel(II) and cobalt(II) ions on Aspergillus fumigatus immobilized Diaion HP-2MG has been investigated. The analytical conditions including amounts of A. fumigatus, eluent type, flow rates of sample and eluent solutions were examined. Good recoveries were obtained to the spiked natural waters. The influences of the concomitant ions on the retentions of the analytes were also examined. The detection limits (3sigma, N = 11) were 0.30 μg l−1 for copper, 0.32 μg l−1 for iron, 0.41 μg l−1 for zinc, 0.52 μg l−1 for lead, 0.59 μg l−1 for nickel and 0.72 μg l−1 for cobalt. The relative standard deviations of the procedure were below 7%. The validation of the presented procedure is performed by the analysis of three standard reference materials (NRCC-SLRS 4 Riverine Water, SRM 1515 Apple leaves and GBW 07605 Tea). The procedure was successfully applied for the determination of analyte ions in natural waters microwave digested samples including street dust, tomato paste, black tea, etc.  相似文献   

17.
Fengkui Wu  Jiagen Lv   《Talanta》2007,72(5):1811-1817
A flow-injection chemiluminescence (CL) method coupled with solvent extraction for the determination of dexamethasone acetate (DA) in ointment was presented in this paper. It was based on the enhancing effect of the studied drug on CL emission of luminol–K3Fe(CN)6 system. This method has the advantages of simple sample treatment, cheap instrumentation and rapid detection. Under the optimum conditions, relative CL intensities were proportional to DA concentrations in the 0.044–4.4 μg ml−1 range. The limit of detection was 0.01 μg ml−1 (3σ) for DA. The method was applied to DA quantification in commercial DA ointment pharmaceutical and to human skin DA absorption analysis. Experiments were performed to evaluate the nature of DA enhanced luminol–K3Fe(CN)6 CL reaction. Based on the experimental results, it was suggested that in this CL system, DA was oxidized by K3Fe(CN)6 to form a medium product (DAox), DAox oxidized luminol with a faster kinetic step comparing with K3Fe(CN)6 oxidized luminol to an active form. As a result, DA speed the luminol CL reaction, and finally intensified the CL signal.  相似文献   

18.
Burakham R  Oshima M  Grudpan K  Motomizu S 《Talanta》2004,64(5):1259-1265
A novel spectrophotometric reaction system was developed for the determination of nitrite as well as nitrate in water samples, and was applied to a flow-injection analysis (FIA). The spectrophotometric flow-injection system coupled with a copperised cadmium reductor column was proposed. The detection was based on the nitrosation reaction between nitrite ion and phloroglucinol (1,3,5-trihydroxybenzene), a commercially available phenolic compound. Sample injected into a carrier stream was split into two streams at the Y-shaped connector. One of the streams merged directly and reacted with the reagent stream: nitrite ion in the samples was detected. The other stream was passed through the copperised cadmium reductor column, where the reduction of nitrate to nitrite occurred, and the sample zone was then mixed with the reagent stream and passed through the detector: the sum of nitrate and nitrite was detected. The optimised conditions allow a linear calibration range of 0.03–0.30 μg NO2-N ml−1 and 0.10–1.00 μg NO3-N ml−1. The detection limits for nitrite and nitrate, defined as three times the standard deviation of measured blanks are 2.9 ng NO2-N ml−1 and 2.3 ng NO3-N ml−1, respectively. Up to 20 samples can be analyzed per hour with a relative standard deviation of less than 1.5%. The proposed method could be applied successfully to the simultaneous determination of nitrite and nitrate in water samples.  相似文献   

19.
A simple GF-AAS method for speciation analysis of chromium in mineral waters and salinas was developed. Cr(VI) species were separated from Cr(III) by solid-phase extraction with APDC (ammonium pyrrolidinedithiocarbamate). The APDC complexes were formed in the sample solution under proper conditions, adsorbed on Diaion HP-2MG resin and the resin was separated from the sample. After elution with concentrated nitric acid Cr(VI) was determined by GF-AAS. Total chromium was determined by GF-AAS directly in the sample and Cr(III) concentration was calculated as the difference between those results.

The detection limit of the method defined as 3 s of background variation was 0.03 μg l−1 for Cr(VI) and 0.3 μg l−1 for total chromium. RSD for Cr(VI) determination at the concentration of 0.14 μg l−1 was 9%, and for total chromium at the concentration of 5.6 μg l−1 was 5%. The recovery of Cr(VI) was in the range of 94–100%, dependently on type of the sample.

The investigation of recovery of the spiked Cr(VI) showed that at concentration levels near 1 μg l−1 and lower recovery may be reduced significantly even by pure reagents that seem to be free from any reductants.  相似文献   


20.
Jin Pan  Yuming Huang  Weiqun Shu  Jia Cao 《Talanta》2007,71(5):1861-1866
At pHs ≥ 11.45, trace Al was found to enhance the CL from luminol–KMnO4 system. However, at pHs ≤ 10.42, it was found to inhibit strongly the CL from luminol–KMnO4 system. The effect of pH, luminol and potassium permanganate concentrations on the kinetic characteristics of CL system was investigated in the presence of trace Al. On this basis, a flow injection inhibition chemiluminescence method was established for the determination of trace Al in this study. Under optimized conditions, the CL decreased linearly with Al(III) concentration in the range of 8–500 μg L−1 and the detection limit (3σ) of 2 μg L−1. The relative standard deviation (R.S.D.) is 3.6% for 100 μg L−1 Al(III) (n = 11). The method has been applied to the determination of trace Al in real water samples with satisfactory results without the pretreatment of samples. The results given by the proposed method are in good agreement with those given by ICP-AES detection method.  相似文献   

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