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1.
A stir foam composed of graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) was prepared for use in micro-solid phase extraction sorbent of preservative agents and antioxidants from cosmetic products. The extracted analytes were quantified by GC-MS. Under the optimized conditions, the calibration plots are linear in the concentration ranges between 5.0 μg·L?1 to 1.0 mg·L?1 for benzoic acid, of 10.0 μg·L?1 to 1.0 mg·L?1 for 2-methyl-3-isothiazolinone (MI), and between 1.0 μg·L?1 and 1.0 mg·L?1 for both 3-tert-butyl-4-hydroxyanisole (BHA) and 2,6-di-tert-butyl-p-hydroxytoluene (BHT). The LODs are 1.0 μg·L?1 for benzoic acid, 5.0 μg·L?1 for MI and 0.5 μg·L?1 for both BHA and BHT. The stir-foam can be easily prepared, is inexpensive and well reproducible (RSDs <3%, for n?=?6). It can be re-used for up to 12 times after which extraction efficiency has dropped to 90%. The method was successfully applied to the determination of preservatives and antioxidants in cosmetic samples. Recoveries from spiked samples ranged between 94.5?±?2.1% and 99.8?±?1.8%.
Graphical abstract A stir foam was prepared from graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) and is shown to be a most viable sorbent for the microextraction of trace amounts of preservative agents and antioxidants from cosmetic products.
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2.
A new chemically modified carbon paste electrode by 2,2?-((pyridine-2,6-diylbis(azanylylidene))bis(methanylylidene))diphenol (L) ligand has been made and used as a sensor for determination of trace mercury and cadmium ions with cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods. Complexation studies of the ligand with Cu2+, Zn2+, Hg2+, Ni2+ and Cd2+ ions by conductometric method in acetonitrile–ethanol mixture at 25°C show that the ML complexes have formed. The formation constants of complexes were calculated from the computer fitting of the molar conductance–mole ratio data, and the stability of the resulting complexes varied in order of Cd2+ > Hg2+ > Cu2+ > Zn2+ > Ni2+. Then a simple and effective chemically modified carbon paste electrode with L was prepared, and the electrochemical properties and applications of the modified electrode were investigated. Under the optimal conditions, the detection limit was 0.0494 μg L?1 and 0.0782 μg L?1 for cadmium and mercury ions, respectively, and the linear range for both metal ions were from 1 to 100 μg L?1. The electrode shows high sensitivity, reproducibility and low cost, and was successfully applied to determination of Cd2+ and Hg2+ ions in water samples with recovery in the range of 97–101%.  相似文献   

3.
《Analytical letters》2012,45(11):1921-1930
This paper describes a simple and sensitive method for the determination of manganese in human urine by graphite furnace atomic absorption spectroscopy (GFAAS), which includes sample preparation by microwave digestion. Matrix modifier combinations, the digestion power, pyrolysis, and atomization temperatures were optimized. A mixture of 5.0 µg Pd(NO3)2 and 3.2 µg Mg(NO3)2 modifier presented the best performance. The optimal temperatures for pyrolysis and atomization were 1500°C and 1950°C, respectively. The GFAAS method was compared to inductively coupled plasma–mass spectrometry (ICP–MS) for the determination of manganese in urine. Analytical figures of merit for GFAAS and ICP–MS were: accuracy (3.46%, 2.19%), precision (3.61%, 5.84%), LOD (0.109 µg · L?1, 0.015 µg · L?1), LOQ (0.327 µg · L?1, 0.045 µg · L?1), and recovery (80–100%, 74–89%). Both methods were employed for the determination of Mn in urine and the results were compared statistically.  相似文献   

4.
Voltammetric procedures for trace metals analysis in polluted natural waters using homemade bare gold-disk microelectrodes of 25- and 125-μm diameters have been determined. In filtered seawater samples, square wave anodic stripping voltammetry (SWASV) with a frequency of 25 Hz is applied for analysis, whereas in unfiltered contaminated river samples, differential pulse anodic stripping voltammetry (DPASV) gave more reliable results. The peak potentials of the determined trace metals are shifted to more positive values compared to mercury drop or mercury-coated electrodes, with Zn always displaying 2 peaks, and Pb and Cd inversing their positions. For a deposition step of 120 s at ?1.1 V, without stirring, the 25-μm gold-disk microelectrode has a linear response for Cd, Cu, Mn, Pb and Zn from 0.2 μg L?1 (1 μg L?1 for Mn) to 20 μg L?1 (30 μg L?1 for Zn, Pb and 80 μg L?1 for Mn). Under the same analytical conditions, the 125-μm gold-disk microelectrode shows linear behaviour for Cd, Cu, Pb and Zn from 1 μg L?1 (5 μg L?1 for Cd) to 100 μg L?1 (200 μg L?1 for Pb). The sensitivity of the 25-μm electrode varied for different analytes from 0.23 (±0.5%, Mn) to 4.83 (±0.9%, Pb) nA L μmol?1, and sensitivity of the 125-μm electrode varied from 1.48 (±0.7%, Zn) to 58.53 (±1.1%, Pb  nA L μmol?1. These microelectrodes have been validated for natural sample analysis by use in an on-site system to monitor Cu, Pb and Zn labile concentrations in the Deûle River (France), polluted by industrial activities. First results obtained on sediment core issued from the same location have shown the ability of this type of microelectrode for in situ measurements of Pb and Mn concentrations in anoxic sediments.   相似文献   

5.
A sensitive, economic, rapid and simple method for the determination of four N-methylcarbamate pesticides: methomyl (2.0–80 μg L?1), aldicarb (5.0–50 μg L?1), butocarboxim (2.0–60 μg L?1) and oxamyl (2.0–60 μg L?1); is reported. It relies on the coupling of photoinduced chemiluminescence (PICL) detection with flow injection (FI) methodology. The automation of FI together with the use of light as a reagent decreased the environmental impact of the analysis. The proposed method was based on the oxidation of these pesticides, previously irradiated on-line with UV light, with cerium(IV), using quinine as a sensitiser. Limits of detection below the legal limits (100 ng L?1) established by the European Union for drinking waters were obtained without the need of preconcentration steps. A good inter-day reproducibility (1.6–6.4%, n = 5), repeatability (rsd = 2.7 %, n = 25) and high throughput (123 h?1) were achieved. The method was successfully applied to the determination of methomyl in natural waters with mean recoveries ranging from 90% to 98%.  相似文献   

6.
We present a method for the separation and determination of transition metals in electrolytes based on ion chromatography (IC) with post-column reaction (PCR) and serial conductivity and spectrophotometric detection. Three IC columns [Metrosep C4—250/4.0 (column A), Metrosep C6—250/4.0 (column B), and Nucleosil 100-5SA—250/4.6 (column C)] with different capacities, and stationary phases were used and compared with each other for method development. All spectrophotometric measurements were carried out with 4-(2-pyridylazo)resorcinol (PAR) as PCR reagent at a wavelength of 500 nm. To characterize the precision of the separation, the selectivity for the analysis of transition metals (nickel, cobalt, copper, and manganese) in the presence of large amounts of lithium and the resolution of the peaks were determined and compared with one another. Furthermore, the limits of detection (LOD) and quantification (LOQ) were determined for the transition metals. The LODs and LOQs determined by column C were as follows: cobalt (LOD/LOQ): 9.4 µg L?1/31.3 µg L?1, manganese (LOD/LOQ): 7.0 µg L?1/23.5 µg L?1, and nickel (LOD/LOQ): 6.3 µg L?1/21.1 µg L?1. Finally, the concentration of transition metal dissolution of the cathode material Li1Ni1/3Co1/3Mn1/3O2 (NCM) was investigated for different charge cut-off voltages by the developed IC method.  相似文献   

7.
《Analytical letters》2012,45(7-8):1172-1189
The purpose of this study consists in reporting of single laboratory validation of a method for the determination of total inorganic arsenic by hydride generation atomic absorption spectrometry from natural and residual water samples. Applicability, fitness for purpose, selectivity, and sensitivity were discussed. A calibration study was realized, linear working range (0.4–4 μg·L?1), detection (0.11 μg·L?1), and quantification (0.38 μg·L?1) limits being determined. It was also proven that the method is accurate and precise. Following the bottom-up approach measurement, uncertainty was estimated (method validation data were used).  相似文献   

8.
Dispersive liquid–liquid microextraction (DLLME) based on the solidification of floating organic droplets (DLLME-SFO) combined with gas chromatography-electron-capture detection (GC–ECD) has been developed for extraction and analysis of three dinitrobenzenes. The extraction conditions including extraction solvent, disperser solvent, extraction time, salt effect and temperature were investigated and optimized systematically. The limits of detection were 0.019 μg L?1 for 1,4-dinitrobenzene, 0.079 μg L?1 for 1,3-dinitrobenzene and 0.034 μg L?1 for 1,2-dinitrobenzene. Moreover, it offered good repeatability and high recovery. This method was successfully applied to monitor DNBs in different water samples.  相似文献   

9.
A novel ZnO-graphene oxide nanocomposite was prepared and is shown to be a viable coating on fused silica fibers for use in solid phase microextraction (SPME) of diazepam and oxazepam from urine, this followed by thermal desorption and gas chromatographic quantitation using a flame ionization detector. A central composite design was used to optimize extraction time, salt percentage, sample pH and desorption time. Limits of detection are 0.5 μg·L?1 for diazepam and 1.0 μg·L?1 for oxazepam. Repeatability and reproducibility for one fiber (n?=?4), expressed as the relative standard deviation at a concentration of 50 μg·L?1, are 8.3 and 11.3% for diazepam, and 6.7 and 10.1% for oxazepam. The fiber-to-fiber reproducibility is <17.6%. The calibration plots are linear in the 5.0–1000 μg·L?1 diazepam concentration range, and from 1.0–1000 μg·L?1 in case of oxazepam. The fiber for SPME has high chemical and thermal stability (even at 280 °C) after 50 extractions, and does not suffer from a reduction in the sorption capacity.
Graphical abstract A hydrothermal method was introduced for preparation of ZnO- GO nano composite on a fused silica fiber as solid phase microextraction with high mechanical, chemical stability and long service life
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10.
《Analytical letters》2012,45(15):2508-2521
Porous polyaniline coatings doped with different counter ions were electrodeposited on the surface of stainless steel wires using controlled potentiostatic coulometry. Prior to electropolymerization, the stainless steel wires were chemically etched to improve subsequent immobilization of the polyaniline coatings on the substrate and to increase the effective surface area. Porous polyaniline coatings doped with sulfate, nitrate, and perchlorate counter ions were employed for solid-phase microextraction (SPME) of 2-chlorophenol, 2,4-dichlorophenol, triclosan, and 2,4-dichlorophenoxyacetic acid coupled to high-performance liquid chromatography. The results demonstrated that the perchlorate doped polyaniline coating exhibited the highest extraction efficiency for 2-chlorophenol, 2,4-dichlorophenol, and triclosan at pH 5.0, indicating that the extraction capability was modified by introducing different counter ions into the coatings. As a result, the perchlorate doped polyaniline coated fiber was further used for the optimization of extraction condition s . The method provided linear dynamic ranges over 2 to 4 orders of magnitude. The limits of detection were 0.006 µg · L?1, 0.005 µg · L?1, and 0.040 µg · L?1 for 2-chlorophenol, 2,4-dichlorophenol, and triclosan, respectively. The precision expressed as the relative standard deviation ranged from 2.20% to 5.04% for spiked water at 10 µg · L ?1 (n = 5) and the fiber to fiber reproducibility was between 3.27% and 5.91% (n = 5). The method was successfully applied to the determination of chlorophenolics in real water samples. The recoveries of chlorophenolics in spiked water at 5.0 µg · L?1 were between 99.60% and 108.7% with relative standard deviations between 3.24% and 5.47%.  相似文献   

11.
A simple and specific method for the simultaneous determination of eleutherosides B and E in powdered rhizomes of Eleutherococcus senticosus extract and in solid and liquid dietary supplements was developed and validated. E. senticosus extracts, often mixed with other plants or herbal extracts, are widely used in food supplements because of the tonic and adaptogenic activities referred to the eleutherosides B and E. In this study, samples were analyzed by a liquid chromatography-electrospray tandem mass spectrometry (LC–ESI-MS/MS) method operated in single reaction monitoring (SRM). Validation was carried out in terms of limit of detection (LOD), limit of quantitation (LOQ), linearity, precision and trueness. LOD and LOQ values were fixed at 3 μg L?1 and 10 μg L?1, respectively, whereas linearity was established within 10–1,000 μg L?1 range for both compounds. Good precision was obtained for both eleutherosides in terms of intra-day precision (RSD % lower than 4 %) and inter-day precision (RSD % lower than 6 %). Good percentage recoveries were obtained for both eleutherosides (91.5–103.6 %). Finally, the developed method was successfully applied to analyze a number of solid and liquid commercial dietary supplements containing E. senticosus extracts, also mixed with other herbal extracts.  相似文献   

12.
《Analytical letters》2012,45(14):2184-2192
A new procedure for trace tungsten W(VI) in soil by fluorescence quenching method coupled with cloud point extraction (CPE) as the separation-preconcentration method was described. The Triton X-100 CPE behavior of W(VI)-salicylfluorone (SAF)was investigated. Under the optimized conditions, the fluorescence quenched intensity (ΔF) was linearly with W(VI). The range of linear was 0.8 ~ 20.0 μg · L?1, the detection limit (DL) was 0.14 ng · mL?1 (3σ), the relative standard deviation 3.3% (c = 10.0 μg · L?1, n = 5) and the recovery was 101.0–102.2%. The proposed method applied to the analysis of W(VI) in certified reference materials and real samples.  相似文献   

13.
Colloidal gold, quantum dots and polystyrene microspheres were used as labels in three kinds of lateral flow immunochromatographic assays (ICAs) for the detection of zearalenone (ZEN) in cereal samples. The assays allow ZEN to be quantified within 20 min. The LODs are 10 μg·L?1 of ZEN for the colloidal gold-based ICA, and 1 μg·L?1 for both the quantum dot and polystyrene microsphere based ICAs. The respective data are 60 μg·kg?1, 6 μg·kg?1 and 6 μg·kg?1, respectively, for spiked samples and cereals. Only minor cross-sensitivity occurred between ZEN and fusarium toxins, and no cross-sensitivity if found for aflatoxin B1, T-2 mycotoxin, ochratoxin A, deoxynivalenol, and fumonisin B1. LODs of the three assays are lower than the maximum limits of ZEN set by most standardization agencies.
Graphical abstract Schematic presentation of three lateral flow immunochromatographic assays (ICAs) based on the use of (a) colloidal gold (CG), (b) fluorescent quantum dots (QD), and (c) polystyrene microspheres (PMs) as signalling labels for the rapid and sensitive determination of zearalenone (ZEN) in cereal samples.
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14.
《Analytical letters》2012,45(17):2747-2757
Abstract

Brazilian sugarcane spirits were analyzed to elucidate similarities and dissimilarities by principal component analysis. Nine aldehydes, six alcohols, and six metal cations were identified and quantified. Isobutanol (LD 202.9 µg L?1), butiraldehyde (0.08–0.5 µg L?1), ethanol (39–47% v/v), and copper (371–6068 µg L?1) showed marked similarities, but the concentration levels of n-butanol (1.6–7.3 µg L?1), sec-butanol (LD 89 µg L?1), formaldehyde (0.1–0.74 µg L?1), valeraldehyde (0.04–0.31 µg L?1), iron (8.6–139.1 µg L?1), and magnesium (LD 1149 µg L?1) exhibited differences from samples.  相似文献   

15.
We report a sensitive and simple method for analysis of traces of Sudan dyes in foods in which solid-phase extraction on activated silica gel for preconcentration was combined, on-line, with high-performance liquid chromatography. With a loading flow rate of 1.7 mL min?1 for sampling 50 mL Sudan I–IV at pH 6.7, enrichment factors ranging from 196 to 991 were achieved. Detection limits (S/N = 3) of Sudan I–IV were in the range 1.4–7.0 ng L?1, and the relative standard deviation for repeatability of peak areas in five replicate analyses of 0.01 μg L?1 Sudan I–IV was 2.2–4.5%. When blank food samples (chilli powder, chilli sauce, and duck eggs) were spiked with Sudan III at two levels (0.25 and 0.50 μg L?1) then analyzed by this method recovery ranged from 70.3 to 95.2%.  相似文献   

16.
A single-drop microextraction (SDME) procedure with a modified microsyringe was developed for the analysis of six organophosphorus pesticides (OPPs) in water. Microsyringe was modified by attaching a 2-mm cone onto the needle tip end. The conditions affecting SDME performance including microextraction solvent, stirring speed, extraction time, ionic strength and sample pH were optimized. Under the optimized conditions, the linear ranges of the SDME with ethion as internal standard were 0.05–50 μg L?1 (except for dimethoate 5–5,000 μg L?1) and limits of detection (LOD) were 0.012–0.020 μg L?1 (except for dimethoate 0.45 μg L?1). Recoveries of six pesticides were in the range of 70.6–107.5 % with relative standard deviation lower than 6.0 %. The modified method is simple, rapid and sensitive, and acceptable in the analysis of OPPs pesticides in water samples.  相似文献   

17.
ABSTRACT

The flow injection catalytic spectrophotometry is proposed for the determination of nitrite based on the catalytic effect on the redox reaction between methylene blue and potassium bromate in acidic medium. The reaction is monitored spectrophotometrically by measuring the decrease in the absorbance of methylene blue at the maximum absorption wavelength of 664 nm. The method is characterised by low solvent consumption and easy automatic continuous analysis. It has higher sensitivity and lower detection limit. Experimental analysis conditions of the flow injection-catalytic photometry are optimised, and the best analysis conditions are: the concentration of the potassium bromate is 0.068 mol L?1; the concentration of the phosphoric acid in oxidation liquid is 0.045 mol L?1; the concentration of the methylene blue in colour-substrate solution is 2.4 mg L?1, the volume of sample ring is 200 μL; the reaction coil is around 7 m in length; the inject time is 50 s and analysis time is 70 s. Under the optimal conditions, the linear range is from 10 to 500 μg L?1 and the detection limit is 1 μg L?1. The nitrate standard solution is continuously determined with a mass concentration of 300 μg L?1. The RSD is determined to be 1.41% (n = 10). The nitrite in water samples, which were from the Half Acre pond, the Ink River and the Small West lake in a campus, was determined respectively by this method. A satisfactory standard addition recovery of 96.7%–103.9% was obtained.  相似文献   

18.
An amino acid derived ionic liquid, Fe3O4 nanoparticles and graphene oxide (GO) were used to prepare a material for the magnetic solid phase extraction (MSPE) of the ions Al(III), Cr(III), Cu(II) and Pb(II). The material was characterized by Fourier transform infrared spectral (FT-IR), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), magnetic analysis and isoelectric point (pI) analysis. It is shown to be a viable sorbent for the separation of these metal ions. Single factor experiments were carried out to optimize adsorption including pH values, ionic strength, temperature and solution volume. Following desorption with 0.1 M HCl, the ions were quantified by inductively coupled plasma optical emission spectrometry. Under the optimum conditions, the method provides a linear range from 10 to 170 μg· L?1 for Al(III); from 4.0 to 200 μg· L?1 for Cr(III); from 5.0 to 170 μg· L?1 for Cu(II); and from 5.0 to 200 μg· L?1 for Pb(II). The limits of detection (LOD) are 6.2 ng L?1 for Al(III); 1.6 ng L?1 for Cr(III); 0.52 ng L?1 for Cu(II); and 30 ng L?1 for Pb(II). Method performance was investigated by determination of these ions in (spiked) environmental water and gave recoveries in the range of 89.1%–117.8%.
Graphical abstract The graph shows that Al(III), Cr(III), Cu(II), Pb(II) are not adsorbed quantitatively by Fe3O4-SiO2. On the other hand, Cr(III) and Pb(II) are adsorbed quantitatively by Fe3O4-SiO2-GO while Al(III) and Cu(II) are not quantitatively retained. However, 3D–Fe3O4-SiO2-GO-AAIL adsorb all these 4 metal ions quantitatively.
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19.
The occurrence of 26 commonly used cytostatic compounds in wastewaters was evaluated using an automated solid-phase extraction (SPE) method with liquid chromatography–high-resolution mass spectrometry (LC–HRMS). Detection was optimized using Oasis HLB SPE cartridges at pH 2. Two hospital effluents and their two receiving wastewater treatment plants were sampled over five days. In hospital effluents, eight cytostatics were detected at levels up to 86.2 μg L?1 for ifosfamide, 4.72 μg L?1 for cyclophosphamide, and 0.73 μg L?1 for irinotecan, the three most relevant compounds identified. Cyclophosphamide and megestrol acetate were found in wastewaters at concentrations up to 0.22 μg L?1 for the latter. The predicted environmental concentrations (PEC) in sewage effluents of ifosfamide (2.4–4.3 ng L?1), capecitabine (11.5–14.2 ng L?1), and irinotecan (0.4–0.6 ng L?1), calculated from consumption data in each hospital, published excretion values for the target compounds, and wastewater elimination rates, were in agreement with experimental values.  相似文献   

20.
Polyimide (PI) sheets were laser etched to obtain graphene-based carbon nanomaterials (LEGCNs). These were analyzed by scanning electron microscopy, X-ray diffraction and Raman spectroscopy which confirmed the presence of stacked multilayer graphene nanosheets. Their large specific surface and large number of edge-plane active sites facilitate the accumulation of metal ions. A glassy carbon electrode (GCE) with an in-situ plated bismuth film was modified with the LEGCNs to give a sensor with satisfactory response for the simultaneous determination of cadmium(II) and lead(II) by means of square wave anodic stripping voltammetry. It appears that is the first report on an electrochemical sensor based on the use of laser etched graphene for determination of heavy metal ions. Figures of merit for detection of Cd(II) include (a) a low and well separated working potential of ?0.80 V (vs. Ag/AgCl), (b) a wide linear range (from 7 to 120 μg·L?1), and a low detection limits 0.47 μg·L?1. The respective data for Pb(II) are (a) -0.55 V, (b) 5 to 120 μg·L?1, and (c) 0.41 μg·L?1. The modified GCE displays remarkable repeatability, reproducibility, selectivity and stability. The sensor was applied to the simultaneous determination of Cd(II) and Pb(II) in spiked real water samples. The results confirm that the laser etching technique is an efficient tool for the preparation of carbon nanomaterials with high quality and great sensing performance.
Graphical abstract Bismuth film and laser etched graphene-modified glassy carbon electrode (BF-LEGCN/GCE) for the simultaneous determination of cadmium(II) and lead(II) by square wave anodic stripping voltammetry.
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