共查询到20条相似文献,搜索用时 234 毫秒
1.
Design of a field flow system for the on-line spectrophotometric determination of phosphate, nitrite and nitrate in natural water and wastewater 总被引:1,自引:0,他引:1
Ioannis A. Tsoulfanidis George Z. Tsogas Dimosthenis L. Giokas Athanasios G. Vlessidis 《Mikrochimica acta》2008,160(4):461-469
This study describes the design and optimisation of a field flow system for the in-situ collection and on-line determination
of phosphate, nitrate and nitrite by flow injection analysis-spectrophotometry. The method is based on the initial determination
of phosphate as its phosphoantimonylmolybdenum blue complex which is then oxidized on-line by nitrite and the decrease in
absorbance is monitored at 880 nm. Nitrate is determined as the difference between total and initial nitrite content in a
separate flow after reduction to nitrite in a cadmium reductive column. The calibration curves were linear in the range 0–2.00 mg L−1 P-phosphate, 0–10.00 mg L−1 nitrite and 0–7.00 mg L−1 nitrate with correlation coefficients of 0.9979, 0.9993 and 0.9995, respectively. The detection limits, calculated as 3S/N,
were 0.15 mg L−1 for P-phosphate, 0.17 mg L−1 for nitrite and 0.09 mg L−1 for nitrate. The reproducibility was below 3.0% (n = 7). Method validation in the analysis of natural water and wastewater samples revealed that it can efficiently be applied
to the determination of the target analytes, with recoveries in the range of 92–108%.
Correspondence: Athanasios G. Vlessidis, Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina,
Ioannina 45110, Greece 相似文献
2.
Paraskevas D. Tzanavaras Demetrius G. Themelis Anastasios Economou Georgios Theodoridis 《Mikrochimica acta》2003,142(1-2):55-62
Two new simple and rapid methods are reported for the accurate and precise spectrophotometric determination of captopril
(CPL) using flow (FI) and sequential injection (SI) analysis. The methods are based on the fast oxidation of CPL by Fe(III).
The produced Fe(II) reacts with 2,2′-dipyridyl-2-pyridylhydrazone (DPPH) in acidic medium to form a colored complex which
is monitored spectrophotometrically at 535 nm. Both methods allow the determination of the analyte up to 1000 mg L−1 at a sampling rate of 120 and 60 injections per hour for FI and SI, respectively. The methods are very precise [s
r=0.8 and 1.2% at 500 mg L−1 CPL (n=12) for FI and SI, respectively] and the 3σ detection limits (c
L=4.0 and 7.0 mg L1, respectively) are quite satisfactory. Their application to a variety of anti-hypertensive commercial pharmaceutical formulations
showed excellent results (relative errors, e
r, < ± 1.6% in all cases compared to an official HPLC method), while common pharmaceutical excipients were found not to interfere.
Recovery experiments further verified the accuracy of the developed methods, as the percent recoveries were in the range of
98.1–102.5%.
Author for correspondence. E-mail: themelis@chem.auth.gr
Received May 9, 2002; accepted January 8, 2003
Published online May 5, 2003 相似文献
3.
María del Mar Cordero-Rando Manuel Barea-Zamora Juan M. Barberá-Salvador Ignacio Naranjo-Rodríguez Juan A. Muñoz-Leyva José L. Hidalgo-Hidalgo de Cisneros 《Mikrochimica acta》1999,132(1):7-11
A zeolite-modified carbon paste electrode (CPE) has been used for the determination of 4-nitrophenol by differential pulse
voltammetry (DPV). The electrochemical reduction of 4-nitrophenol at −1.0 V is carried out in a Britton-Robinson medium at
pH 3.5. The cyclic voltammetric (CV) behaviour has been investigated to study the nature of the process. Studies on the effect
of pH were carried out over the pH range 2–9 with the Britton-Robinson buffer solution, and the influence of pH on peak height
and peak potential was analyzed. A linear relationship between peak intensity and concentration is obtained in the range 0.2–10 mg L−1, with a detection limit of 0.04 mg L−1; a relative standard deviation of 1.5% for a 5 mg L−1 4-nitrophenol concentration and a relative error of 2.6% were also obtained (n=11).
Received March 3, 1998. Revision December 10, 1998. 相似文献
4.
Jorge L. Guzmán Mar Leticia López Martínez Pedro L. López de Alba Jesús E. Castrejón Durán Víctor Cerdà Martín 《Mikrochimica acta》2006,153(3-4):139-144
1-Naphthylamine (NPA) is one of the main degradation products of pesticides derived from naphthalene, and a well-known bladder
carcinogen in men. The Griess assay is used for NPA determination because of its high sensitivity and selectivity. The azo
dye 4-(sulphophenylazo)-1-naphthylamine is formed, which shows a peak maximum at 540 nm. After optimizing multisyringe flow
injection analysis (MSFIA) parameters, the analytical characteristics of the method were obtained, with a working linear range
of 0.5 to 14 mg L−1, according to the equation A = 0.0738±0.0019 [NPA] + 0.0028 ± 0.0042, r = 0.9997. Values for RSD (%) and Erel (%) were calculated for the concentration levels of 0.5, 6 and 12 mg L−1; values obtained were 1.1, 0.4 and 0.3% for RSD and 0.8, 0.3 and 0.2% for Erel, respectively. LD was 0.01 mg L−1 and LQ was 0.04 mg L−1 NPA. The MSFIA procedure for the determination of NPA was applied to different water samples (well water, tap water, seawater,
and wastewater from the EDAR-1, Palma de Mallorca water treatment plant), with satisfactory results and a throughput of 90
samples per hour. 相似文献
5.
Dimitrios V. Stergiou Spyros C. Karkabounas Panayotis G. Veltsistas Nicholaos P. Evmiridis Athanasios G. Vlessidis 《Mikrochimica acta》2007,158(1-2):59-64
A kinetic-potentiometric method is described for the quantitative assay of formaldehyde (HCHO) in pharmaceutical and industrial
preparations. It is based on the reaction of HCHO with (ethylenediamine)-Cu(II)-sulfate [Cu(CH2NH2)2(H2O)2] · SO4. The changes in potential, resulting from the release of the Cu(II) cations, are monitored with a Cu(II)-ion selective electrode.
The calibration curve for the HCHO is linear in the concentration range 50–250 mg L−1, with a limit of detection of 8.5 mg L−1. The method shows very good reproducibility with an RSD of 2.6% for successive injections (n = 5) of 150 mg L−1 HCHO primary solution, while it is interference free. The method was successfully tested in various industrial and pharmaceutical
preparations. 相似文献
6.
A micro extraction – spectrophotometric procedure is developed for the determination of bismuth in pharmaceutical formulations.
The procedure is based on the extraction of tetraiodobismuthate(III) ion paired with benzyltributylammonium cation into chloroform.
The application of Nile Blue as internal standard (IS) enabled good analytical performance for micro-scale analysis. The ratio
between the absorbances measured at 491 nm (bismuth complex) and at 632 nm (IS) was taken as the analytical signal. The procedure
was carried out in Eppendorf tubes, lowering significantly the use of reagents and the volume of organic solvent. In the calibration
range up to 60 mgċl−1, the linear regression coefficient was 0.9999, the CV for 15 mgċl−1 and for 50 mgċl−1 Bi were 1.6% and 0.7% respectively. The results obtained in the analysis of pharmaceutical formulations were in good agreement
with the results of EDTA titration method.
Received November 25, 1999. Revision February 14, 2000. 相似文献
7.
Jeff E. Prest Sara J. Baldock Peter R. Fielden Nicholas J. Goddard Bernard J. Treves Brown 《Mikrochimica acta》2005,151(3-4):223-230
A new method allowing the simultaneous determination of arsenic(V), selenium(IV) and selenium(VI) using miniaturised isotachophoresis
has been developed. The method uses 0.02 M nitric acid buffered to pH 5.5 with histidine as the leading electrolyte. Using
a miniaturised poly(methyl methacrylate) chip device with an integrated conductivity detector, separations of model samples
and an industrial process stream sample were achieved. Limits of detection were calculated to be 0.85 mg L−1 for arsenic(V), 0.95 mg L−1 for selenium(IV) and 1.0 mg L−1 for selenium(VI). A method for the analysis of arsenic(III), using a glycolic acid based leading electrolyte to eliminate
carbonate interference is also presented. 相似文献
8.
Abdel-Aziz Youssef El-Sayed Ebtesam Ahmad Saad Basheer Mohamed Mohamed Ibrahime Mohamed Tarek Mohamed Zaki 《Mikrochimica acta》2000,135(1-2):19-27
Simple, rapid, sensitive and selective methods for the determination of Cr(III) and W(VI) with flavonol derivatives in the
presence of surface-active agents are proposed. In the pH ranges 3.4–4.2 and 1.9–2.5, the molar absorptivities of Cr(III)-morin-emulsifier
S (EFA) and W(VI)-morin-polyvinylpyrrolidone (PVP) systems are 1.13×105 and 2.13×104 L mol−1 cm−1 at 435 and 415 nm, respectively. The Cr(III)-quercetin-PVP and W(VI)-quercetin-cetylpyridinium bromide (CPB) systems are
formed in the pH ranges 4–4.6 and 2.2–2.8 with molar absorptivities 1.02×105 and 9.02×104 L. mol−1 cm−1 at 441 and 419 nm, respectively. The linear dynamic ranges for the determination of Cr(III) and W(VI) with morin in the presence
of EFA and PVP are 0.03–0.46 and 0.71–8.1 μg mL−1, respectively. The corresponding ranges with quercetin are 0.04–0.54 and 0.14–2.1 μg mL−1 of Cr(III) and W(VI), respectively. The r.s.d (n = 10) for the determination of 0.25 and 3.7 μg mL−1 of Cr(III) and W(VI) with morin and their detection limits are 0.88 and 0.99% and 0.016 and 0.63 μg mL−1, respectively. Using quercetin, the r.s.d (n = 10) for 0.22 and 1.2 μg mL−1 of Cr(III) and W(VI) and their detection limits are 0.92 and 0.91% and 0.015 and 0.08 μg mL−1, respectively. The critical evaluation of the proposed methods is performed by statistical analysis of the experimental data.
The proposed methods are applied to determine Cr in steel, non-ferrous alloys, wastewater and mud filtrate and to the determination
of W in steel.
Received March 8, 1999. Revision January 21, 2000. 相似文献
9.
Leonardo Sena Gomes Teixeira Antônio Celso Spínola Costa Júlio César Rosa Assis Sérgio Luis Costa Ferreira Mauro Korn 《Mikrochimica acta》2001,137(1-2):29-33
A new sensitive method exploiting solid-phase spectrophotometry is proposed for the determination of cobalt in pharmaceutical
preparations. The chromogenic reagent 1-(2-thiazolylazo)-2-naphthol (TAN) was immobilized on C18 bonded silica loaded into
a home-made cell with 1.5 mm of optical path for cobalt determination. Cobalt(II) reacts with TAN on C18 material, at pH 6.0–7.5,
to give a coloured complex which has maximum absorption at 572 nm. In this way, the sample was passed through the cell and
Co(II) ions were quantitatively retained on the solid-phase. After the direct measurement of light-absorption in the solid
phase, only the cobalt was eluted with 0.1 mol L−1 hydrochloric acid. The cell was washed with water and then another sample solution could be passed through the cell. The
procedure allowed the determination of cobalt in the range of 10–160 μg L−1 with coefficient of variation of 4.7% (n=10) and apparent molar absorptivity of 2.62 × 106 L mol−1 cm−1 using sample volume of 3-mL.
Received May 15, 2000. Revision August 28, 2000. 相似文献
10.
Citric acid was thermochemically esterified onto defatted cotton fibre to produce a carboxyl cotton chelator (CCC), which
had been used for extraction of copper prior to its determination by flame atomic absorption spectrometry. The extraction
of copper has been studied under both batch and column methods. Quantitative extraction of copper was achieved in the pH range
4–7. The time needed to extract each sample was less than 30 min by the batch method. The copper extraction capacity of CCC
was found to be 22.7 mg g−1 at optimal pH value. The elution was quantitative with 1 mol L−1 hydrochloric acid. The feasible flow rate of copper-containing solution for quantitative extraction onto the column packed
with CCC was 0.5–4.0 mL min−1, whereas for elution it was less than 1.5 mL min−1. A 100-fold extraction factor could be achieved under the optimal column conditions. The tolerance limits for common metal
ions on the extraction of copper and the time of column reuse were investigated. The proposed method has been successfully
applied for extraction and determination of copper in industrial wastewater and natural water samples. 相似文献
11.
A new adsorbent is proposed for the solid-phase extraction of phenol and 1-naphthol from polluted water. The adsorbent (TX-SiO2) is an organosilica composite made from a bifunctional immobilized layer comprising a major fraction (91%) of hydrophilic
diol groups and minor fraction (9%) of the amphiphilic long-chain nonionic surfactant Triton X-100 (polyoxyethylated isooctylphenol)
(TX). Under static conditions phenol was quantitatively extracted onto TX-SiO2 in the form of a 4-nitrophenylazophenolate ion associate with cetyltrimethylammonium bromide. The capacity of TX-SiO2 for phenol is 2.4 mg g−1 with distribution coefficients up to 3.4 × 104 mL g−1; corresponding data for 1-naphthol are 1.5 mg g−1 and 3 × 103 mL g−1. The distribution coefficient does not change significantly for solution volumes of 0.025–0.5 L and adsorbent mass less than
0.03 g; 1–90 μg analyte can be easily eluted by 1–3 mL acetonitrile with an overall recovery of 98.2% and 78.3% for phenol
and 1-naphthol, respectively. Linear correlation between acetonitrile solution absorbance (A
540) and phenol concentration (C) in water was found according to the equation A
540 = (6 ± 1) × 10−2 + (0.9 ± 0.1)C (μmol L−1) with a detection range from 1 × 10−8 mol L−1 (0.9 μL g−1) to 2 × 10−7 mol L−1 (19 μL g−1), a limit of quantification of 1 μL g−1 (preconcentration factor 125), correlation coefficient of 0.936, and relative standard deviation of 2.5%. A solid-phase colorimetric
method was developed for quantitative determination of 1-naphthol on adsorbent phase using scanner technology and RGB numerical
analysis. The detection limit of 1-naphthol with this method is 6 μL g−1 while the quantification limit is 20 μL g−1. A test system was developed for naked eye monitoring of 1-naphthol impurities in water. The proposed test kit allows one
to observe changes in the adsorbent color when 1-naphthol concentration in water is 0.08–3.2 mL g−1. 相似文献
12.
A new Schiff-base ligand [N, N′, N″-Tri- (2,4-dihydroxyacetophenone) – triaminotriethylamine (TDATA)] with a tripodal structure
was synthesized. Its fluorescence intensity with the europium(III) complex was increased about 178-fold in the presence of
sodium acetate (NaAc) and about 126-fold in the presence of sodium phosphate (Na3PO4) solution. After adding the organic solvent dimethylsulfoxide (DMSO) to the above system, which leads to Eu3+ the fluorescence was further enhanced about 12-fold. Spectrofluorimetric determination of trace amounts of Eu3+ based on the phenomenon was performed. The excitation and emission wavelength is 365 nm and 615 nm, respectively. Under optimum
conditions, the fluorescence intensities vary linearly with the concentration of Eu3+ in the range of 4.9 × 10−12–3.2 × 10−6 mol · L−1 with a detection limit of 4.5 × 10−12 mol · L−1 (for the TDATA-NaAc-DMSO system) or 6.2 × 10−11–8.6 × 10−6 mol · L−1 with a detection limit of 6.0 × 10−11 mol · L−1 (for the TDATA-Na3PO4-DMSO system). Interferences of some rare earth metals and other inorganic ions are described. The method is a selective,
sensitive, rapid and simple analytical procedure for the determination of europium(III) in a high purity yttrium oxide and
synthetic sample. The mechanism for the fluorescence enhancement is also discussed. 相似文献
13.
Nabila M. Guindy Zeinab M. Abou-Gamra Michel F. Abdel-Messih 《Monatshefte für Chemie / Chemical Monthly》2000,131(8):857-866
Summary. The kinetics of the formation of the 1:3 complex of chromium(III) with L-glutamic acid and DL-lysine were studied spectrophotometrically at and 550 nm. The reaction was found to be first order in both reactants. Increasing the hydrogen ion concentration from 3.2×10−5 to 1.0×10−3 molċdm−3 retarded the reaction rate which is of the form . Values of 28.8 and 63.6 kJċmol−1 were obtained for the energy of activation and −184 and −116 Jċ K−1ċmol−1 for the entropy of activation for L-glutamic acid and DL-lysine. The logarithms of the formation constants of the two complexes were found to be 5.9 and 5.1.
Received January 7, 2000. Accepted (revised) March 8, 2000 相似文献
14.
Ilona Šperlingová Ludmila Dabrowská Vladimír Stránský Šárka Dušková Jan Kučera Monika Tvrdíková Milon Tichy 《Analytical and bioanalytical chemistry》2010,397(2):433-438
Ethylene glycol monobutyl ether (EGBE), an industrial solvent, is absorbed by the body not only by inhalation but also by
dermal absorption (liquid or vapour). EGBE is metabolized to butoxyacetic acid (BAA). Pooled freeze-dried urine candidate
reference material (RM) was prepared from urine obtained from persons occupationally exposed to EGBE. This material has the
advantage of containing butoxyacetic acid in both the free and conjugated (glutamine and glycine) forms, as found in native
urine. In all GC method modifications used, acid hydrolysis was used to release BAA from its conjugated form. The amount of
butoxyacetic acid in homogeneity and stability testing was measured by GC after derivatisation with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide. Detection was by MS in EI mode, in the authors’ laboratory. For interlaboratory comparison of the
reference material GC methods with MS, FID, and ECD were used. Different extraction solvents (dichloromethane–isopropanol
2:1, ethyl acetate, or dichloromethane) and derivatisation reagents (trimethylsilyldiazomethane, N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide) were used. Using ANOVA (at the statistical level α = 0.05) no changes were found in the concentration of butoxyacetic acid during fifteen month isochronous stability testing,
or in homogeneity testing. The uncertainty contributions were u
h = 8.8 mg L−1 and u
s = 6.5 mg L−1. The concentration of butoxyacetic acid in freeze-dried urine RM was evaluated from the results of eight laboratory data
sets within an interlaboratory comparison by use of the interactive statistical software IPECA. The contribution to total
uncertainty derived from interlaboratory comparison was u
i = 12.7 mg L−1. The reference value (c = 273 ± 33 mg L−1) is an unweighted arithmetic average of accepted results. The value is traceable to the pure butoxyacetic acid (98% w/w; Acros Organic #257760010) used as calibrant. The uncertainty given is combined expanded uncertainty derived from the results
from interlaboratory comparison, and from homogeneity and stability tests (k = 2). The reference material will be used to verify method performance in the biological monitoring of occupational exposure
to EGBE. 相似文献
15.
Silica gel was prepared by the sol–gel method, modified with nanometer-sized zirconium oxide, and this material was characterized
by X-ray diffraction. A micro-column packed with silica gel modified with nanometer zirconium oxide as sorbent has been developed
for the quantitative separation and preconcentration of trace amounts of chromium(III) prior to their determination by electrothermal
atomic absorption spectrometry. Total chromium was determined after the reduction of chromium(VI) to chromium(III) by 10%
(m/v) of aqueous ascorbic acid as reducing reagent. The adsorption capacity for chromium(III) was found to be 2.36 mg g−1. The detection limit for chromium(III) was 15 ng L−1 with an enrichment factor of 100. The relative standard deviation was 3.2% (n = 7, c = 2.0 ng mL−1). 相似文献
16.
Thermally two-dimensional lattice graphene (GR) and biocompatibility chitosan (CS) act as a suitable support for the deposition
of palladium nanoparticles (PdNPs). A novel hydrogen peroxide (H2O2) biosensor based on immobilization of hemoglobin (Hb) in thin film of CS containing GR and PdNPs was developed. The surface
morphologies of a set of representative membranes were characterized by means of scanning electron microscopy and showed that
the PdNPs are of a sphere shape and an average diameter of 50 nm. Under the optimal conditions, the immobilized Hb showed
fast and excellent electrocatalytic activity to H2O2 with a small Michaelis–Menten constant of 16 μmol L−1, a linear range from 2.0 × 10−6 to 1.1 × 10−3 mol L−1, and a detection limit of 6.6 × 10−7 mol L−1. The biosensor also exhibited other advantages, good reproducibility, and long-term stability, and PdNPs/GR–CS nanocomposites
film would be a promising material in the preparation of third generation biosensor. 相似文献
17.
An approach for rapid quantitation of 5-hydroxymethylfurfural (HMF) in honey using planar chromatography is suggested for
the first time. In high-performance thin-layer chromatography (HPTLC) the migration time is approximately 5 min. Detection
is performed by absorbance measurement at 290 nm. Polynomial calibration in the matrix over a range of 1:80 showed correlation
coefficients, r, of ≥ 0.9997 for peak areas and ≥ 0.9996 for peak heights. Repeatability in the matrix confirmed the suitability of HPTLC–UV
for quantitation of HMF in honey. The relative standard deviation (RSD, %, n = 6) of HMF at 10 ng/band was 2.9% (peak height) and 5.2% (peak area); it was 0.6% and 1.0%, respectively, at 100 ng/band.
Other possible detection modes, for example fluorescence measurement after post-chromatographic derivatization and mass spectrometric
detection, were also evaluated and can coupling can be used as an additional tool when it is necessary to confirm the results
of prior quantitation by HPTLC–UV. The confirmation is provided by monitoring the HMF sodium adduct [M + Na]+ at m/z 149 followed by quantitation in TIC or SIM mode. Detection limits for HPTLC–UV, HPTLC–MS (TIC), and HPTLC–MS (SIM) were 0.8 ng/band,
4 ng/band, and 0.9 ng/band, respectively. If 12 μL honey solution was applied to an HPTLC plate, the respective detection
limits for HMF in honey corresponded to 0.6 mg kg−1. Thus, the developed method was highly suitable for quantitation of HMF in honey at the strictest regulated level of 15 mg kg−1. Comparison of HPTLC–UV detection with HPTLC–MS showed findings were comparable, with a mean deviation of 5.1 mg kg−1 for quantitation in SIM mode and 6.1 mg kg−1 for quantitation in TIC mode. The mean deviation of the HPTLC method compared with the HPLC method was 0.9 mg kg-1 HMF in honey. Re-evaluation of the same HPTLC plate after one month showed a deviation of 0.5 mg kg−1 HMF in honey. It was demonstrated that the proposed HPTLC method is an effective method for HMF quantitation in honey.
相似文献
18.
Rodrigues TH Rocha MV de Macedo GR Gonçalves LR 《Applied biochemistry and biotechnology》2011,164(6):929-943
In this work, the potential of microwave-assisted alkali pretreatment in order to improve the rupture of the recalcitrant
structures of the cashew able bagasse (CAB), lignocellulosic by-product in Brazil with no commercial value, is obtained from
cashew apple process to juice production, was studied. First, biomass composition of CAB was determined, and the percentage
of glucan and lignin was 20.54 ± 0.70% and 33.80 ± 1.30%, respectively. CAB content in terms of cellulose, hemicelluloses,
and lignin, 19.21 ± 0.35%, 12.05 ± 0.37%, and 38.11 ± 0.08%, respectively, was also determined. Results showed that, after
enzymatic hydrolysis, alkali concentration exerted influence on glucose formation, after pretreatment with 0.2 and 1.0 mo L−1 of NaOH (372 ± 12 and 355 ± 37 mg gglucan−1) when 2% (w/v) of cashew apple bagasse pretreated by microwave-assisted alkali pretreatment (CAB-M) was used. On the other hand, pretreatment
time (15–30 min) and microwave power (600–900 W) exerted no significant effect on hydrolysis. On enzymatic hydrolysis step,
improvement on solid percentage (16% w/v) and enzyme load (30 FPU gCAB-M−1) increased glucose concentration to 15 g L−1. The fermentation of the hydrolyzate by Saccharomyces cerevesiae resulted in ethanol concentration and productivity of 5.6 g L−1 and 1.41 g L−1 h−1, respectively. 相似文献
19.
Arroyo-Manzanares N García-Campaña AM Gámiz-Gracia L 《Analytical and bioanalytical chemistry》2011,401(9):2987-2994
Ochratoxin A (OTA) is a mycotoxin naturally found in various foods, including wine. As OTA is considered as a possible human
carcinogen, the maximum concentration for this compound has been established at 2 μg kg−1 in wine by the EU (Directive (CE) No 1881/2006). Typically, immunoaffinity columns have been used for its extraction. However,
simpler, more efficient and less contaminant extraction systems are demanding. In this work, dispersive liquid–liquid microextraction
using ionic liquid as extractant solvent (IL-DLLME) and the QuEChERS procedure, have been evaluated and compared for extraction
of OTA in wine samples. Laser-induced fluorescence (LIF, He–Cd Laser excitation at 325 nm) coupled with capillary HPLC has
been used for the determination of OTA, using a sodium dodecyl sulfate micellar solution in the mobile phase to increase the
fluorescence intensity. Matrix-matched calibration curves were established for both methods, obtaining LODs (3× S/N) of 5.2 ng·L−1 and 85.7 ng·L−1 for IL-DLLME and QuEChERS, respectively. Clean extracts were obtained for white, rose and red wines with both methods, with
recoveries between 88.7–94.2% for IL-DLLME and between 82.6–86.2% for QuEChERS. The precision was evaluated in terms of repeatability
(n = 9) and intermediate precision (n = 15), being ≤ 8.5% for IL-DLLME and ≤ 5.4% for QuEChERS. 相似文献
20.
CeO2 nanoparticles approximately 12 nm in size were synthesized and subsequently characterized by XRD, TEM and UV-vis spectroscopy.
Then, a gold electrode modified with CeO2 nanoparticles was constructed and characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV).
The modified electrode demonstrated strong catalytic effects with high stability towards electrochemical oxidation of rutin.
The anodic peak currents (measured by differential pulse voltammetry) increased linearly with the concentration of rutin in
the range of 5.0 × 10−7–5.0 × 10−4 mol · L−1. The detection limit (S/N = 3) was 2.0 × 10−7 mol · L−1. The relative standard deviation (RSD) of 8 successive scans was 3.7% for 5.0 × 10−6 mol · L−1 rutin. The method showed excellent sensitivity and stability, and the determination of rutin in tablets was satisfactory. 相似文献