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1.
ABSTRACT

In this work, a novel layered sorbent for microextraction by packed sorbent (MEPS) was introduced, which has been prepared by coating graphene oxide/polyamide (GO/PA) nanocomposite (NC) onto cellulose paper through solvent exchange method. Scanning electron microscopy (SEM) was applied to investigate the surface characteristic and morphology of PA and GO/PA NC coated on cellulose paper. The prepared MEPS device was used for extraction of organophosphorous pesticides (OPPs) including chlorpyrifos, fenthion, fenithrothion, ethion, edifenphos and phosalone in environmental aqueous samples followed by detection using gas chromatography-flame ionisation detector (GC-FID). Important parameters affecting the MEPS method including pH of sample solution, extraction draw-discard cycles, sorbent layers, desorption solvent volume and desorption draw-eject number were studied and optimised using central composite design (CCD). Based on the method validation, limits of detection (LODs) were in the range of 0.2–1 µg L?1. The calibration graphs for chlorpyrifos, fenthion and edifenphos are linear in the concentration range of 1 to 500 µg L?1; for ethion and phosalone are linear in the range of 1–1000 µg L?1 and for fenithrothion is linear in the range of 3–1000 µg L?1. The method precision (RSD %) with six replicates determinations was in the range of 3 to 9.4 % and 3.9 to 11.9% for distilled water and spiked river water sample, respectively, at the concentration level of 300 µg L?1 . The developed method was applied successfully to determine OPP compounds in river, dam and tap water samples; accordingly, the relative recoveries (RR%) were obtained in the range of 77.8 to 113.3%.  相似文献   

2.
In this work, magnetic solid-phase extraction based on sodium dodecyl sulfate-coated Fe3O4 nanoparticles has been successfully applied for extraction and preconcentration of trace amounts of nystatin from water and vaccine samples prior to high-performance liquid chromatography–ultraviolet detection. Various experimental parameters affecting extraction and recovery of the analyte, such as the amount of sodium dodecyl sulfate, pH of the sample solution, salt concentration, extraction time, sample volume and desorption conditions, were systematically studied and optimized. Under optimized conditions, nystatin was quantitatively extracted. Proper linear range with good coefficient of determination, (R 2 > 0.99) and limit of detection and quantification (based on signal-to-noise ratios of 3 and 10) of 2.0 and 5.0 µg L?1, over the investigated concentration range (5–700 µg L?1), were obtained, respectively. The intra-day and inter-day relative standard deviations at 50 µg L?1 level of NYS were 1.4 and 4.5% based on six replicate determinations. The accuracy of the method was evaluated by recovery measurements on spiked samples. Suitable recoveries of 96–102 and 26–44% were achieved (at spiked levels of 50, 300 and 500 µg L?1) for water and vaccine samples, respectively.  相似文献   

3.
In this paper, a novel molecularly imprinted polymer coated stir bar has been used to selectively extract naphthalene sulfonates (NSs) directly from seawater sample. 1-Naphthalene sulfonic acid (1-NS) was used as template molecule. The effects of different parameters were optimized on the extraction efficiency and the optimum conditions were established as: the absorption and desorption times were fixed, respectively, at 10 and 15 min, stirring speed was 700 rpm, pH was adjusted to 4.1, amount of NaCl was 1 mol L?1 and extraction process was performed at a temperature of 50 °C. The linear ranges were 2–250 µg L?1 for 3,6-NDS-1-OH (1-naphthol-3,6-disulfonic acid), 4–250 µg L?1 for 2-NS (2-naphthalene sulfonate) and 3–250 µg L?1 for 1-NS. The detection limits were within the range of 0.32–0.95 µg L?1. Under optimum conditions, the detection limits of the NSs were 0.84, 0.95 and 0.32 µg L?1 with the enrichment factor of 117-, 41- and 77-fold for 2-NS, 1-NS, and 6-NDS-1-OH, respectively. The repeatability of the method was satisfactory (0.53 ≤ RSD ≤6.0 %, n = 10). The method has been successfully applied for the analysis of trace amounts of three naphthalene sulfonates in seawater of Chabahar Bay.  相似文献   

4.
In the existing study, a new vortex-assisted cloud point extraction (VA-CPE) method was developed for determination of low levels of thiosulfate in environmental waters at 632 nm by spectrophotometry. The method is selectively based on charge-transfer-sensitive ion-pair complex formation of Ag(S2O3)2 3?, which is produced by the reaction of thiosulfate with excess Ag+ ions with toluidine blue (3-amino-7-dimethylamino-2-methylphenazathionium chloride, TB+) and then its extraction into micellar phase of polyethylene glycol 4-tert-octylphenyl ether (Triton X-45) in presence of Na2SO4 as salting-out agent at pH 7.0. All the factors affecting complex formation and VA-CPE efficiency were optimized in detail. Under the optimized conditions, the linear calibration curves for thiosulfate were in the range of 0.2–120 and 5–180 µg L?1 with sensitivity improvement of 81-folds and 15-folds, respectively, as a result of efficient mass transfer obtained by CPE with and without vortex, while it changed in the range of 260–3600 µg L?1 without preconcentration at 642 nm. The limits of detection and quantification of the method for VA-CPE were found to be 0.05 and 0.22 µg L?1, respectively. The precision (expressed as the percent relative standard deviation) was in range of 2.5–4.8% (5, 10 and 25 µg L?1, n: 5). The method accuracy was validated by comparing the results to those of an independent 5,5′-dithiobis(2-aminobenzoic acid) (DTNB) method as well as recovery studies from spiked samples. It has been observed that the results are statistically in a good agreement with those obtained by DTNB method. Finally, the method developed was successfully applied to the preconcentration and determination of trace thiosulfate from environmental waters.  相似文献   

5.
In the present study, a simple versatile extraction method based on supramolecular solvent microextraction followed by inductively coupled plasma atomic emission spectrometry was developed for the extraction, separation and determination of zirconium (Zr) from hafnium (Hf). Zr and Hf were complexed with bis(2,4,4-trimethylpentyl) phosphinic acid, to obtain hydrophobic complex, and extracted into supramolecular solvent phase. The effective parameters on the supramolecular solvent microextraction efficiency were studied and optimized by using two different optimization methods: one variable at a time and central composite design. Under the optimum conditions, the linear range of 0.3–200.0 and 2.0–200.0 µg L?1, detection limits (S/N = 3) of 0.1 and 0.6 µg L?1, and precisions (n = 5) of 3.2–4.9% and 3.0–5.1% were obtained for Zr and Hf, respectively. Finally, the proposed method has been successfully applied for the extraction and separation of these cations in zirconium ore sample.  相似文献   

6.
A novel and efficient sulfadiazine imprinted polymer was synthesized via co-precipitation method and successfully grafted on magnetic multi-walled carbon nanotubes. The synthesized magnetic imprinted polymer was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction analysis, thermal analysis and applied as a sorbent for selective magnetic solid-phase extraction of sulfadiazine. The retained sulfadiazine was eluted by 150.0 µL methanol/acetic acid (6:4) solution and quantified by fiber optic linear array spectrophotometry via formation of a detectable azo dye. All parameters affecting the extraction of sulfadiazine were investigated and optimized. Under the optimized conditions, the method exhibited a linear dynamic range of 2.0–50.0 µg L?1 with a detection limit of 0.56 µg L?1 and enrichment factor of 300.0. The relative standard deviation at 30.0 µg L?1 of sulfadiazine (N = 6) was 2.8 and 4.6% for intra-day and inter-day, respectively. The method was successfully applied to determine sulfadiazine in human urine, honey, milk and environmental water samples.  相似文献   

7.
A rapid, simple, and efficient method using ultrasound-assisted emulsification microextraction combined with dispersive micro-solid phase extraction (USAE-D-µ-SPE) was developed for detection and quantification of three azole antifungals in milk samples by high-performance liquid chromatography diode array detector. In this study, mesoporous carbon, COU-2, was used as sorbent in USAE-D-µ-SPE for the extraction and preconcentration of analytes. Several important experimental parameters, including type of deproteinized solvents, desorption time, type of extraction solvents, volume of extraction solvent, extraction time, emulsification time, sample pH, salt addition, and mass of COU-2 sorbent, were optimized using spiked milk samples. Under the optimum extraction and detection conditions, three azole antifungals, namely ketoconazole, clotrimazole, and miconazole, were determined within 20 min, with good linearity of matrix-matched calibration in the range of 0.5–5000.0 µg L?1 with coefficient of determination, r 2 ≥ 0.9943. The method showed limits of detection and limits of quantification of all analytes in the range of 0.15–3.0 and 0.5–10.0 µg L?1, respectively. Good repeatability with RSDs <15% (n = 3) and satisfactory relative recoveries (83.3–111.1%) were obtained for spiked azole antifungal drugs in milk. The results reveal that the developed USAE-D-µ-SPE method was a simple, rapid, efficient, environmentally friendly, and practicable method for the determination of azole antifungals in milk samples.  相似文献   

8.
A fast and simple ultrasound-assisted dispersive liquid–liquid microextraction method for determination of Sodium Closantel has been developed. High-performance liquid chromatography with ultraviolet detector has been used for the determination of Sodium Closantel. The effect of influencing parameters such as type and volume of extraction and disperser solvents, pH of sample solution, extraction time and amount of salt was also investigated. Optimization of method was performed using Plackett–Burman experimental design and surface response methodology. Under the optimal conditions, the linear dynamic range of Sodium Closantel was from 10 to 3000 µg L?1 with a correlation coefficient of 0.997 and a detection limit of 1.0 µg L?1. The relative standard deviation was less than 3.5% (n = 5). The method has been successfully applied for determination of Sodium Closantel in real samples. The enrichment factor was 48 under optimal conditions.  相似文献   

9.
An SPE-HPTLC method for simultaneous identification and quantification of seven pharmaceuticals in production wastewater was optimized and validated. The studied compounds were enrofloxacine, oxytetracycline, trimethoprim, sulfamethazine, sulfadiazine, sulfaguanidine and penicillin G/procaine. The method involves solid-phase extraction on hydrophilic-lipophilic balance cartridges with methanol and HPTLC analysis of extracts on CN modified chromatographic plates followed by videodensitometry at 254 and 366 nm. Optimization of chromatographic separation was performed by systematic variation of the mobile phase composition using genetic algorithm approach and the optimum mobile phase composition for TLC separation was 0.05 M H2C2O4:methanol = 0.81:0.19 (v/v). Linearity of the method was demonstrated in the ranges from 1.5 to 15.0 μg L−1 for enrofloxacine, 100–500 μg L−1 for oxytetracycline, 150–600 μg L−1 for trimethoprim, 300–1100 μg L−1 for sulfaguanidine and 100–400 μg L−1 for sulfamethazine, sulfadiazine and penicillin G/procaine with coefficients of determination higher than 0.991. Mean recoveries ranged from 74.6 to 117.1% and 55.1 to 108.0% for wellspring water and production wastewater, respectively. Only sulfaguanidine showed lower results. The described method has been applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.  相似文献   

10.
Liquid phase microextraction with back extraction (LPME-BE) combined with liquid chromatography-ultra violet (LC-UV) was applied for the extraction and determination of methadone in biological fluids. At the optimized conditions, an enrichment factor of 386 and detection limit (LOD) of 0.2 μg L?1 were obtained. The calibration curve was linear (r 2 = 0.989) in the concentration range of 0.6–1,000 μg L?1. Within-day relative standard deviation RSD (S/N = 3) and between-day RSD were 2.7 and 5.9%, respectively. The feasibility of the proposed method was evaluated by extraction and determination of methadone in plasma and urine samples and satisfactory results were obtained.  相似文献   

11.
A selective separation and preconcentration method for the determination of gold ions in water and ore samples has been developed using dispersive liquid–liquid microextraction, followed by flame atomic absorption spectrometry. 4-Ethyl-1(2-(4-(4-nitrophenyl)piperazin-1-yl)acetyl)thiosemicarbazide) (NPPTSC) has been used for the first time as new chelating reagent. A mixture of ethanol (dispersive solvent) and carbon tetrachloride (extraction solvent) was used. Some parameters affecting the extraction procedure including the type and volume of the extracting and dispersive solvents, HNO3 concentration, the chelating agent amount, volume of sample, and foreign ions have optimized. Also, the complex formation between gold ions and the ligand has been investigated in a methanol–water solution (1:1) using UV–visible spectrometry. The spectrophotometric titration data showed that of Au–NPPTSC complex composition was found to be 3:2. After optimizing the instrumental and experimental parameters, we achieved a detection limit of 1.5 µg L?1, a preconcentration factor of 50, and a linear dynamic range of 10.0–400.0 µg L?1. The relative standard deviation obtained 2.1% at 50 µg L?1 for gold ions (n = 10). The proposed method was successfully performed for the determination of gold in certified reference material, environmental water, and ore samples.  相似文献   

12.
《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   

13.
A vortex-assisted dispersive liquid–liquid microextraction method in combination with UV–Vis spectrophotometry was developed for the simultaneous extraction and determination of iron species. In this method, Fe2+ and Fe3+ were complexed with pyridine-2-amidoxime, neutralized through ion pair formation with sodium dodecyl sulfate, and extracted into the fine droplets of chloroform. After centrifugation, the absorbance of the extracted complexes was recorded in the wavelength range of 360–700 nm. The parameters affecting the extraction efficiency such as the pH, the type and volume of the extraction solvent, ligand concentration, and sample volume were optimized. The individual iron species was then determined by means of the orthogonal signal correction–generalized partial least squares method. Under the optimized conditions, the calibration curves were linear over the range of 2.0–100 and 3.0–200 µg L?1 with detection limits of 0.4 µg L?1 for Fe2+ and 0.8 µg L?1 for Fe3+, respectively. The relative standard deviations for intra- and inter-day assays (n = 5) were 2.3 and 4.0 for Fe2+ at 50 µg L?1 and 2.7 and 4.3 for Fe3+ at 30 µg L?1, respectively. The enhancement factors of 77 and 69 were achieved for Fe2+ and Fe3+, respectively. The proposed method was successfully applied to the determination of iron species in water samples.  相似文献   

14.
Formaldehyde is known as a highly toxic compound to humans and identified as a carcinogenic substance. In this study, Hantzsch reaction was utilized for the derivatization of trace amounts of formaldehyde in aqueous samples with acetylacetone in the presence of ammonia to form an extractable colored product named 3,5-diacetyl 1,4-dihydrolutidine (DDL) and its further extraction using two-phase hollow fiber liquid-phase microextraction. The main experimental variables affecting the extraction performance were investigated and optimized. Under the optimum conditions (sample volume 12 mL; reaction temperature 70 °C; ammonium acetate buffer solution 4 mL 0.1 mol L?1; acetylacetone 5 mL 0.15 mol L?1; solvent octanol, salt concentration 20% (w/v) NaCl; pH of donor phase 7.0; stirring speed 400 rpm and extraction time 30 min), the linear dynamic range, limit of detection (LOD as 3S b/m) and relative standard deviation (RSD %) of the proposed method were obtained as 5–250 μg L?1 (r 2 = 0.9979), 3.6 μg L?1 and 2.5%, respectively. Finally, the applicability of the proposed method was examined, and very good results were obtained. The results confirmed the applicability of the proposed method as a versatile, low-cost and sensitive preconcentration method for determination of low concentrations of formaldehyde in aqueous solutions.  相似文献   

15.
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   

16.
《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   

17.
《Analytical letters》2012,45(13):2075-2088
For the first time, a simple method for magnetic stirring-assisted dispersive suspended microextraction has been developed for the determination of three fungicides (azoxystrobin, diethofencarb, and pyrimethanil) in water and wine samples. The method is based on the solidification of a floating organic droplet coupled with high performance liquid chromatography. In the proposed method, the low toxicity solvent 1-dodecanol was used as the extractant. Both the extraction and phase separation process were performed with magnetic stirring. No centrifugation step was involved. After separating the two phases, the extraction solvent droplet was easily collected through solidification at lower temperature. Important parameters such as the kind and volume of organic extraction solvent, extraction and restoration speed, extraction and restoration time, and salt concentration were optimized. Under the optimal conditions, the limits of detection for the analytes varied from 0.14 to 0.26 µg L?1. The enrichment factors ranged from 125–200. The linearity ranges were 1–2000 µg L?1, yielding correlation coefficients (r) higher than 0.9990. The relative standard deviation (n = 6) at two spiked level of 0.2 µg mL?1 and 4 µg L?1 varied between 2.2% and 7.8%. Finally, the developed technique was successfully applied to determine target fungicides in real water and wine samples, where the obtained recoveries ranged from 83.8–105.3%  相似文献   

18.
In this work, a new method based on homogeneous liquid-phase microextraction was developed for the determination of methadone and tramadol. Dipropylamine was used as extraction solvent with switchable hydrophilicity that can be miscible/immiscible upon the addition or removal of CO2 as a reagent. The effects of operational parameters of the extraction such as volume of acceptor phase, volume of donor phase, pH of donor phase, and ionic strength of solution were investigated. Under optimal conditions, the preconcentration factors, the detection limits and the linearity of the method were achieved in the ranges of 135–138, 1.2 and 4–1000 µg L?1, respectively. Finally, the proposed method has been successfully applied to the analysis of methadone and tramadol in urine samples. In urine sample, the preconcentration factors were 118 and 122 for methadone and tramadol, respectively. Additionally, calibration curves were found to be linear in the concentration range of 8–1000 µg L?1 with the r2 values better than 0.998. In addition, limits of detection and quantification were 2.4 and 8 µg L?1, respectively, for both analytes.  相似文献   

19.
Simultaneous analysis of homotaurine and its homologous, taurine, is a highly challenging issue, especially in matrices they exist simultaneously. A simple precolumn derivatization procedure combined with high-performance liquid chromatography–fluorescence detection was developed for simultaneous determination of homotaurine and taurine in marine macro-algae. The analytes were derivated with o-phthalaldehyde at an ambient temperature and alkaline medium. Calibration curves were linear in the ranges of 50–2500 µg L?1 for homotaurine and 100–2500 µg L?1 for taurine with the coefficients of determination higher than 0.998. Limits of detection of homotaurine and taurine were 15 and 30 µg L?1, respectively. Intraday (n = 6) and inter-day (n = 4) precisions of the method were satisfactory with relative standard deviations less than 6.0%. Good recoveries (>94%) were acquired by the method for extraction of homotaurine and taurine from algae matrices. Liquid chromatography–mass spectrometry was also used to confirm detection of the analytes in algae samples. The data suggest that the method was successfully applied to simultaneous determination of homotaurine and taurine in algae samples.  相似文献   

20.
《Analytical letters》2012,45(14):1995-2005
Using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM][PF6]) ionic liquid as extraction solvent, five estrogens including estrone (E1), 17β-estradiol (E2), estriol (E3), 17α -ethynylestradiol (EE2), and diethylstilbestrol (DES) in water samples were determined by dispersive liquid-liquid microextraction (DLLME) followed by high performance liquid chromatography with a photodiode array detector and a fluorescence detector (HPLC-DAD-FLD). The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of [C6MIM][PF6] dispersed entirely into the sample solution with the help of a disperser solvent (acetone). Parameters including both extraction and disperser solvents and their volumes, extraction and centrifugal time, sample pH, and salt effect were investigated and optimized. Under the optimized conditions, 110–349 fold enrichment factors of analytes were obtained. The calibration curves were linear in the concentration range of 0.2–100 µg L?1 for E2, E3, and EE2 detected with FLD, and 1–100 µg L?1 for E1 and DES detected with DAD. The correlation coefficient of the calibration curve was between 0.9990 and 0.9997. The limits of detection (LOD, S/N = 3) for the five estrogens were in the range of 0.08–0.5 µg L?1. The relative standard deviations (RSD) for six replication experiments at the concentration of 5.0 µg L?1 were ≤5.7%. The proposed method was applied to the analysis of three water samples from different sources (river water, waste water, and sea water). The relative recoveries of spiked water samples are satisfied with 89.3–102.4% and 88.7–105.2% at two different concentration levels of 5.0 and 50.0 µg L?1, respectively.  相似文献   

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