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Find video protocols related to scientific articles indexed in Pubmed.
Determination of benzimidazole anthelmintics in milk and honey by monolithic fiber-based solid-phase microextraction combined with high-performance liquid chromatography-diode array detection.
Anal Bioanal Chem
PUBLISHED: 08-09-2014
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A porous poly(methacrylic acid-co-ethylene dimethacrylate) monolithic fiber (MEMF) for solid-phase microextraction (SPME) of five benzimidazole anthelmintics was prepared by in-situ polymerization. The effect of polymerization conditions on SPME of the target analytes was studied thoroughly. The physicochemical properties of the monolith were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated and, under the optimized conditions, a simple and sensitive method for the determination of trace benzimidazoles residues in milk and honey was established by coupling MEMF-SPME with high-performance liquid chromatography-diode array detection (MEMF-SPME-HPLC-DAD). Under the optimum experimental conditions, the limits of detection (S/N = 3) of the method were 0.11-0.30 ?g L(-1) for milk and 0.086-0.28 ?g L(-1) for honey. Evaluation of intra-day and inter-day precision showed reproducibility was satisfactory-relative standard deviations (RSD) for both were <10 %. Finally, the method was successfully used for determination of benzimidazole residues in milk and honey. Recoveries obtained for determination of benzimidazole anthelmintics in spiked samples ranged from 72.3 to 121 %, with RSD always <11 %.
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[Determination of nitrofuran residues in feed and water samples by monolith-based stir bar sorptive extraction and high performance liquid chromatography].
Se Pu
PUBLISHED: 07-30-2014
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A simple, efficient and sensitive method for the simultaneous determination of nitrofurantoin (NFT), furazolidone (FZD) and nitrofurazone (NFZ) in feed and water samples was developed by stir bar sorptive extraction (SBSE) coupled to high performance liquid chromatography with diode array detection. The SBSE based on poly (vinylimidazole-divinylbenzene) (VIDB) monolithic material as coating was used to concentrate the three target analytes. To obtain the optimum extraction performance, several VIDB-SBSE parameters were investigated and studied, including pH value, ionic strength of sample matrix, extraction and desorption time. Under the optimized experimental conditions, the linear ranges were 0.5-200 microg/L for FZD, 0.25-200 microg/L for NFT and NFZ. The limits of detection (S/N = 3) were in the range of 0.068-0.11 microg/L for the three analytes. The precision of the proposed method was evaluated in terms of intra- and inter-day repeatability calculated as RSD, and it was found that the RSDs were all below 6%. The developed method was successfully applied to the determination of nitrofuran residues in animal feed and water samples. The satisfactory recoveries of the spiked target compounds were in the range of 80.6%-108%.
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Preparation of stir cake sorptive extraction based on polymeric ionic liquid for the enrichment of benzimidazole anthelmintics in water, honey and milk samples.
Anal. Chim. Acta
PUBLISHED: 04-05-2014
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In this work, a new stir cake sorptive extraction (SCSE) using polymeric ionic liquid monolith as sorbent was prepared. The sorbent was obtained by in situ copolymerization of an ionic liquid, 1-allyl-3-methylimidazolium bis[(trifluoro methyl)sulfonyl]imide (AMII) and divinylbenzene (DB) in the presence of N,N-dimethylformamide. The influence of the content of ionic liquid and the porogen in the polymerization mixture on extraction performance was studied thoroughly. The physicochemical properties of the polymeric ionic liquid were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The usefulness of SCSE-AMIIDB was demonstrated by the enrichment of trace benzimidazole anthelmintics. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of trace benzimidazoles residues in water, milk and honey samples was established by coupling SCSE-AMIIDB with high performance liquid chromatography/diode array detection (SCSE-AMIIDB-HPLC/DAD). Results indicated that the limits of detection (S/N=3) for target compounds were 0.020-0.072 ?g L(-1), 0.035-0.10 ?g L(-1) and 0.026-0.076 ?g L(-1) in water, milk and honey samples, respectively. In addition, an acceptable reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSD) of less than 9% and 11%, respectively. Finally, the established AMII-SCSE-HPLC/DAD method was successfully applied for the determination of benzimidazoles residues in milk, honey and environmental water samples. Recoveries obtained for the determination of benzimidazole anthelmintics in spiking samples ranged from 70.2% to 117.6%, with RSD below 12% in all cases.
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Preparation of a new sorbent based on boronate affinity monolith and evaluation of its extraction performance for nitrogen-containing pollutants.
J Chromatogr A
PUBLISHED: 03-18-2014
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In this study, a new boronate affinity sorbent based on poly(4-vinylphenylboronic acid-divinylbenzene) monolith (VPB-DB) was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). The effect of the preparation parameters in the polymerization mixture on extraction performance was investigated thoroughly. The sorbent was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The determination of 8 sulfonamides in environmental water samples with the combination of SCSE and high performance liquid chromatography tandem mass spectrometry detection was selected as a paradigm for the evaluation of extraction performance of poly(VPB-DB) monolith for nitrogen-containing pollutants. Under the optimal extraction conditions, the limits of detection (S/N=3) and limits of quantification (S/N=10) for the target analytes were 0.0012-0.010 and 0.0040-0.033?g/L, respectively. The method also showed good linearity, repeatability, recoveries and high feasibility. At the same time, aromatic amines, nitrophenols, amide herbicides and sudan dyes were also used to evaluate the extractive performance of the sorbent for nitrogen-containing compounds. Results well indicate that the interaction of boron-nitrogen coordination between sorbent and analytes plays a key role in the extraction of nitrogen-containing compounds.
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Preparation of monolithic fibers for the solid-phase microextraction of chlorophenols in water samples.
J Sep Sci
PUBLISHED: 02-08-2014
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Monolithic fibers were synthesized and applied for the solid-phase microextraction and determination of chlorophenols in environmental water samples by coupling with HPLC. The fibers were prepared by copolymerization of vinylimidazole and ethylene dimethacrylate as functional monomer and cross-linker, respectively. The effect of the preparation conditions of monolithic fibers on the extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury-intrusion porosimetry, and SEM were used to characterize the monolithic material. The effect of the extraction parameters, including desorption solvent, extraction and desorption time, pH values, and ionic strength in sample matrix on the extraction performance was investigated thoroughly. Under the improved extraction conditions, the linear ranges of 2-chlorophenol, 2,4-dichlorophenol and pentachlorophenol were 1.0-200 ?g/L and 2.0-200 ?g/L for 2,4,6-trichlorophenol. The detection limits (S/N = 3) were in the range of 0.16-0.45 ?g/L, the RSDs for intraday and interday precisions were <7.0%. Finally, the proposed method was successfully used to detect different environmental water samples. The recoveries of spiked water samples were ranged from 90.0 to 115%. At the same time, satisfactory repeatability was achieved with RSDs < 9.0%.
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Loop flow analysis of dissolved reactive phosphorus in aqueous samples.
Talanta
PUBLISHED: 02-06-2014
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The current flow based method for the determination of dissolved reactive phosphorus (DRP) suffers interference from salinity (e.g. index refractive difference) and the incidentally formed bubbles, which can be a problem for optical detection. Here we reported a simple and robust loop flow analysis (LFA) method for accurate measurement of DRP in different aqueous samples. The chemistry is based on the classic phosphomolybdenum blue (PMB) reaction and the PMB formed in a novel cross-shaped flow cell was detected at 700 nm using a miniature spectrophotometer. The effects of reagents on the kinetic formation of PMB were evaluated. The detection limit was 32 nM with an optical pathlength of 1cm and the relative standard deviations for repetitive determinations of 1, 2 and 8 µM phosphate solutions were 1.8% (n=113, without any stoppage during repeating analysis for >7h), 1.0% (n=49) and 0.39% (n=9), respectively. The analysis time was 4 min sample(-1). The effects of salinity and interfering ions (silicate and arsenate) were evaluated and showed no interference under the proposed protocol for DRP analysis. Using the LFA method, different aqueous samples with a salinity range of 0-34 were analyzed and the results showed excellent agreement with the reference method (slope 0.9982±0.0063, R(2)=0.9987, n=34). Recoveries for spiked samples varied from 95.4% to 103.7%. The proposed method showed insignificant interference from salinity, silicate and arsenate, higher reproducibility, easier operation and was free of the bubble problem.
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Speciation and detection of arsenic in aqueous samples: a review of recent progress in non-atomic spectrometric methods.
Anal. Chim. Acta
PUBLISHED: 01-27-2014
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Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005-2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been made beyond what is in the officially prescribed compendia (which are included) and recent reviews are available.
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Multiple monolithic fiber solid-phase microextraction: a new extraction approach for aqueous samples.
J Chromatogr A
PUBLISHED: 01-25-2014
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A novel multiple monolithic fiber solid-phase microextraction (MMF-SPME) was designed and prepared. Two steps were involved in the preparation of MMF-SPME. Firstly, single thin fiber (0.5mm in diameter) was prepared by co-polymerization of vinylimidazole and ethylene dimethacrylate. Secondly, several thin fibers were bound together to obtain the MMF assembly. The extraction and desorption dynamics of MMF-SPME with different numbers of fibers were studied in detail. In order to demonstrate the usability of the new MMF-SPME, the extraction performance of MMF-SPME for 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol was investigated in direct SPME mode. Results indicated that aqueous samples could form convection effectively within MMF-SPME because there were gaps between fibers. The extraction procedure was accelerated by the convection. At the same time, the MMF-SPME possessed high extraction capacity because more sorbent was employed. Under the optimized extraction conditions, low detection limits (S/N=3) and quantification limits (S/N=10) for the target analytes were achieved within the range of 0.13-0.29 ?g/L and 0.44-0.98 ?g/L, respectively. The MMF-SPME also showed a very long lifespan and good repeatability. Finally, the MMF-SPME was successfully applied to the analysis of tap, lake and ground water samples with spiked recoveries in the range of 73.8-101%.
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Automated spectrophotometric analyzer for rapid single-point titration of seawater total alkalinity.
Environ. Sci. Technol.
PUBLISHED: 09-11-2013
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An automated analyzer was developed to achieve fast, precise, and accurate measurements of seawater total alkalinity (AT) based on single-point titration and spectrophotometric pH detection. The single-point titration was carried out in a circulating loop, which allowed the titrant (hydrochloric acid and bromocresol green solution) and a seawater sample to mix at a constant volume ratio. The dissolved CO2 in the sample-titrant mixture was efficiently removed by an inline CO2 remover, which consists of a gas-permeable tubing (Teflon AF2400) submerged in a sodium hydroxide (NaOH) solution. The pH of the mixture was then measured with a custom-made spectrophotometric detection system. The analyzer was calibrated against multiple certified reference materials (CRMs) with different AT values. The analyzer features a sample throughput time of 6.5 min with high precision (±0.33-0.36 ?mol kg(-1); n = 48) and accuracy (-0.33 ± 0.99 ?mol kg(-1); n = 10). Intercomparison to a traditional open-cell AT titrator showed overall good agreement of 0.88 ± 2.03 ?mol kg(-1) (n = 22). The analyzer achieved excellent stability without recalibration over 11 days, during which time 320 measurements were made with a total running time of over 40 h. Because of its small size, low power consumption requirements, and its ability to be automated, the new analyzer can be adapted for underway and in situ measurements.
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Vertical distribution of total mercury and methylmercury in sediment of the Fugong mangrove area at Jiulong River Estuary, Fujian, China.
Water Environ. Res.
PUBLISHED: 07-10-2013
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The concentrations and vertical distributions of total mercury (Hg) and methylmercury (methyl Hg) in the sediment of the Fugong mangrove area, located at the Jiulong River Estuary, Fujian, China, were investigated. The concentrations of total mercury were between 0.12-0.17 and 0.11-40.14 microg/g, while concentrations of methylmercury were between 0.15-1.8 and 0.081-0.58 ng/g (as mercury), in the dry and rainy seasons, respectively. The total mercury concentration was not correlated with the sampling depth. As the depth increased, methylmercury concentrations first increased to their maximum level at a depth of 10-25 cm, and then decreased; this was similar to the vertical distribution characteristics of methylmercury/total mercury ratios. The mangrove ecosystem was considered as a source of methylmercury for adjacent areas, due to the higher average methylmercury concentration in the mangrove sediment than other sediments nearby. Statistically significant logarithmic correlations, conic correlations, and negative correlations were observed for methylmercury and sulfide concentration, sediment organic matter, and sediment pH, respectively.
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Simultaneous determination of nanomolar nitrite and nitrate in seawater using reverse flow injection analysis coupled with a long path length liquid waveguide capillary cell.
Talanta
PUBLISHED: 06-18-2013
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A reverse flow injection analysis (rFIA) method coupled with 1m liquid waveguide capillary cell and spectrophotometric detection for simultaneous determination of nanomolar nitrite and nitrate in seawater was developed. The design of two analytical channels sharing the same detection system in the proposed method allowed the analysis of both nitrite and nitrate with single sample injection. Different strategies of reagent injection were investigated to obtain a higher sensitivity and a better peak shape. A dual-wavelength detection mode was chosen to eliminate the light source shifting and sample matrix interference. Experimental parameters were optimized based on a univariate experimental design and the matrix effect from seawater was preliminarily investigated. The proposed method had high sensitivity with detection limit of 0.6 nmol L(-1) for both nitrite and nitrate. The linearity was 2-500 nmol L(-1) for both analytes, and the upper limit could be extended by choosing a lower sensitivity detection wavelength. The analytical results of 26 surface seawater samples obtained with the proposed method showed good agreement with those using a reference method operated using an automated segmented flow analyzer. The proposed method could greatly minimize the trouble introduced by bubbles in the segmented flow analyzer. It also had the advantages of high precision and high sample throughput (nitrite and nitrate detected in triplicate; 5 h(-1)). Compared to normal flow injection analysis, the rFIA method is superior due to its lower reagent consumption, less dispersion of sample, as well as higher sensitivity.
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Preparation a new sorbent based on polymeric ionic liquid for stir cake sorptive extraction of organic compounds and inorganic anions.
J Chromatogr A
PUBLISHED: 06-01-2013
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A new multi-interaction sorbent (MIS) based on polymeric ionic liquid was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). In the presence of dimethyl sulfoxide, an ionic liquid, 1-vinylbenzyl-3-methylimidazolium chloride was used as monomer to copolymerize in situ with divinylbenzene to form the MIS. The influences of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance were investigated thoroughly. The MIS was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. Parabens and aromatic amines were used to investigate the extraction performance of MIS-SCSE for apolar and strongly polar analytes, respectively. The extraction parameters for parabens and aromatic amines were optimized. At the same time, simple and sensitive analytical methods for parabens and aromatic amines in real samples were developed by the combination of MIS-SCSE and HPLC/DAD. Some inorganic anions, such as F(-), Br(-), NO3(-), PO4(3-) and SO4(2-), were used to test the extraction performance of MIS-SCSE for anions. Results indicated that mechanism involved in the extraction of MIS is the multi-interaction modes including ?-?, hydrophobic, hydrogen-bonding, dipole-dipole and anion-exchange interactions.
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A sensitive flow-batch system for on board determination of ultra-trace ammonium in seawater: Method development and shipboard application.
Anal. Chim. Acta
PUBLISHED: 05-28-2013
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Combining fluorescence detection with flow analysis and solid phase extraction (SPE), a highly sensitive and automatic flow system for measurement of ultra-trace ammonium in open ocean water was established. Determination was based on fluorescence detection of a typical product of o-phthaldialdehyde and ammonium. In this study, the fluorescence reaction product could be efficiently extracted onto an SPE cartridge (HLB, hydrophilic-lipophilic balance). The extracted fluorescence compounds were rapidly eluted with ethanol and directed into a flow cell for fluorescence detection. Compared with the common used fluorescence method, the proposed one offered the benefits of improved sensitivity, reduced reagent consumption, negligible salinity effect and lower cost. Experimental parameters were optimized using a univariate experimental design. Calibration curves, ranging from 1.67 to 300nM, were obtained with different reaction times. The recoveries were between 89.5 and 96.5%, and the detection limits in land-based and shipboard laboratories were 0.7 and 1.2nM, respectively. The relative standard deviation was 3.5% (n=5) for an aged seawater sample spiked with 20nM ammonium. Compared with the analytical results obtained using the indophenol blue method coupled to a long-path liquid waveguide capillary cell, the proposed method showed good agreement. The method had been applied on board during a South China Sea cruise in August 2012. A vertical profile of ammonium in the South East Asia Time-Series (SEATS, 18° N, 116° E) station was produced. The distribution of ammonium in the surface seawater of the Qiongdong upwelling in South China Sea is also presented.
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Flow injection analysis of trace chromium (VI) in drinking water with a liquid waveguide capillary cell and spectrophotometric detection.
Environ Monit Assess
PUBLISHED: 04-30-2013
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Hexavalent chromium (Cr(VI)) is an acknowledged hazardous material in drinking waters. As such, effective monitoring and assessment of the risks posed by Cr(VI) are important analytical objectives for both human health and environmental science. However, because of the lack of highly sensitive, rapid, and simple procedures, a relatively limited number of studies have been carried out in this field. Here we report a simple and sensitive analytical procedure of flow injection analysis (FIA) for sub-nanomolar Cr(VI) in drinking water samples with a liquid core waveguide capillary cell (LWCC). The procedure is based on a highly selective reaction between 1, 5-diphenylcarbazide and Cr(VI) under acidic conditions. The optimized experimental parameters included reagent concentrations, injection volume, length of mixing coil, and flow rate. Measurements at 540 nm, and a 650-nm reference wavelength, produced a 0.12-nM detection limit. Relative standard deviations for 1, 2, and 10 nM samples were 5.6, 3.6, and 0.72 % (n?=?9), and the analysis time was <2 min sample(-1). The effects of salinity and interfering ions, especially Fe(III), were evaluated. Using the FIA-LWCC method, different sources of bottled waters and tap waters were examined. The Cr(VI) concentrations of the bottled waters ranged from the detection limit to ?20 nM, and tap waters collected from the same community supply had Cr(VI) concentration around 14 nM.
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Quantification, morphology and source of humic acid, kerogen and black carbon in offshore marine sediments from Xiamen Gulf, China.
J Environ Sci (China)
PUBLISHED: 04-20-2013
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Three types of macromolecular organic matters (MOMs), i.e. humic acid (HA), kerogen+black carbon (KB), and black carbon (BC) were extracted from marine sediments of Xiamen Gulf, southeast of China. The chemical composition, morphological property and source of the three extractions were characterized by elemental analyzer/isotope ratio mass spectrometry (EA/IRMS) and scanning electron microscope (SEM). The results showed that KB was the predominant fraction in MOMs, which accounted for 61.79%-89.15% of the total organic content (TOC), while HA consisted less than 5%. The relative high contents of kerogen and BC, and low contents of HA in the samples indicated that anthropogenic input might be the major source of organic matter in marine sediments near the industrial regions. The characterization of SEM, not only revealed morphological properties of the three fractions, but also allowed a better understanding of the source of MOMs. The delta13C values of the three fractions suggested that materials from terrestrial C3 plants were predominant. Furthermore, the anthropogenic activities, such as the discharge of sewage, coal and biomass combustion from industry nearby and agricultural practices within drainage basin of the Jiulong River, were remarkably contributed to the variations in delta13C values of MOMs in the offshore marine sediments.
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Development of monolith-based stir bar sorptive extraction and liquid chromatography tandem mass spectrometry method for sensitive determination of ten sulfonamides in pork and chicken samples.
Anal Bioanal Chem
PUBLISHED: 04-09-2013
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A highly sensitive method was developed for the simultaneous determination of ten sulfonamides in pork and chicken samples by monolith-based stir bar sorptive extraction (SBSE) coupled to high-performance liquid chromatography tandem mass spectrometry. The samples were freeze-dried and extracted by acetonitrile, then enriched and further extracted by SBSE which was based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) as coating. To achieve optimum extraction performance of SBSE for sulfonamides, several parameters, including pH value and ionic strength in the sample matrix and extraction and desorption time, were investigated in detail. Under the optimal conditions, the limits of detection (S/N?=?3) for target sulfonamides were 1.2-6.1 ng/kg in pork and 2.0-14.6 ng/kg in chicken, respectively. Real samples spiked at the concentration of 0.5 and 5.0 ?g/kg showed recoveries above 55% and relative standard deviations below 12%. At the same time, the extraction performances of target sulfonamides on SBSE-VPMB were compared with other SBSE based on porous monolith and commercial SBSE.
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Preparation of magnetic poly(vinylimidazole-co-divinylbenzene) nanoparticles and their application in the trace analysis of fluoroquinolones in environmental water samples.
J Sep Sci
PUBLISHED: 04-04-2013
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Nanosized spherical magnetic poly(vinylimidazole-co-divinylbenzene) particles were synthesized and used as a sorbent for the enrichment of trace fluoroquinolones (FQs) from environmental water samples. A suspension polymerization procedure was used to prepare the sorbent. The magnetic sorbent was characterized by SEM, transmission electron microscopy, elemental analysis, and FTIR spectroscopy. Analysis of enrofloxacin, marbofloxacin, fleroxacin, lomefloxacin, and sparfloxacin in environmental water samples by the combination of the magnetic sorbent and HPLC with diode array detection was selected as a paradigm for the practical application of the new adsorbent. Several extraction conditions, including desorption solvent, extraction and desorption time, pH value, and ionic strength in sample matrix, were optimized. Results showed that the new sorbent had high affinity for FQs and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the target analytes, within the ranges of 0.20-1.46 and 0.68-4.84 ?g/L, respectively. Method repeatability was achieved in terms of intra- and interday precisions, indicated by the RSDs, which were both <10.0%. The method also showed good linearity, simplicity, practicality, and environmental friendliness for the extraction of FQs. Finally, the developed method was successfully applied to the determination of FQs in lake water, surface water, and reservoir water samples. Acceptable recoveries of spiked target compounds in these water samples were in the range of 52.1-104.5%.
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Preparation of stir cake sorptive extraction based on poly(4-vinylbenzoic acid-divinylbenzene) monolith and its application in sensitive determination of ?-agonists in milk and swine urine samples.
J. Hazard. Mater.
PUBLISHED: 03-26-2013
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In this study, a new stir cake sorptive extraction (SCSE) based on poly(4-vinylbenzoic acid-divinylbenzene) (VBADB) monolith was prepared. The effect of preparation conditions of monolith on extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury intrusion porosimetry and scanning electron microscopy were used to characterize the monolithic material. The combination of SCSE-VBADB with high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) detection was developed for sensitive determination of ultra-trace ?-agonists in milk and swine urine samples. In order to obtain the optimal extraction conditions of SCSE-VBADB for ?-agonists, several extractive parameters, including pH values and ionic strength in sample matrix, extraction and desorption time were optimized. Under the optimum conditions, the limits of detection (S/N=3) for the target analytes were 0.007-0.030 ?g/L in milk and 0.002-0.011 ?g/L in swine urine, respectively. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of both <10.0%, respectively. Finally, the proposed method was successfully used to detect ?-agonists in different milk and swine urines samples. Acceptable recoveries ranged from 50.3% to 113% and 50.1% to 92.2% for milk and swine urine samples, respectively; and the RSDs for reproducibility were less than 8.0% for target analytes in all real samples.
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The distribution and sea-air transfer of volatile mercury in waste post-desulfurization seawater discharged from a coal-fired power plant.
Environ Sci Pollut Res Int
PUBLISHED: 03-19-2013
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The waste seawater discharged in coastal areas from coal-fired power plants equipped with a seawater desulfurization system might carry pollutants such as mercury from the flue gas into the adjacent seas. However, only very limited impact studies have been carried out. Taking a typical plant in Xiamen as an example, the present study targeted the distribution and sea-air transfer flux of volatile mercury in seawater, in order to trace the fate of the discharged mercury other than into the sediments. Samples from 28 sampling sites were collected in the sea area around two discharge outlets of the plant, daily and seasonally. Total mercury, dissolved gaseous mercury and dissolved total mercury in the seawater, as well as gaseous elemental mercury above the sea surface, were investigated. Mean concentrations of dissolved gaseous mercury and gaseous elemental mercury in the area were 183 and 4.48 ng m(-3) in summer and 116 and 3.92 ng m(-3) in winter, which were significantly higher than those at a reference site. Based on the flux calculation, the transfer of volatile mercury was from the sea surface into the atmosphere, and more than 4.4 kg mercury, accounting for at least 2.2 % of the total discharge amount of the coal-fired power plant in the sampling area (1 km(2)), was emitted to the air annually. This study strongly suggested that besides being deposited into the sediment and diluted with seawater, emission into the atmosphere was an important fate for the mercury from the waste seawater from coal-fired power plants.
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Sensitive monitoring of penicillin antibiotics in milk and honey treated by stir bar sorptive extraction based on monolith and LC-electrospray MS detection.
J Sep Sci
PUBLISHED: 02-04-2013
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In the present study, a convenient and sensitive method for determination of six penicillin antibiotics (amoxicillin, ampicillin, penicillin G, oxacillin, cloxacillin, and dicloxacillin) in milk and honey samples was developed. Milk and honey samples were diluted with water, then directly treated by stir bar sorptive extraction based on poly (vinylimidazole-divinylbenzene) monolithic material as coating. The analytes were analyzed by LC/ESI- MS/MS. Several extraction parameters including extraction and desorption time, pH value, and ionic strength in sample matrix were investigated in detail. Under the optimized extraction conditions, the calculated detection limits for the target compounds were as low as 0.23-2.66 ng/kg in milk and 0.18-1.42 ng/kg in honey, respectively. Good linearity was obtained for analytes with the correlation coefficients (R(2)) above 0.997. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of <5.0 and <10.0%, respectively. Finally, the proposed method was successfully applied to the determination of penicillin antibiotics residues in different milk and honey samples.
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Sensitive determination of organic acid preservatives in juices and soft drinks treated by monolith-based stir cake sorptive extraction and liquid chromatography analysis.
Anal Bioanal Chem
PUBLISHED: 01-11-2013
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A simple, efficient, and sensitive method for simultaneous determination of sorbic acid (SA), benzoic acid (BA), and cinnamic acid (CA) in juices and soft drinks was developed by stir cake sorptive extraction (SCSE) coupling to high-performance liquid chromatography with diode array detection. The SCSE based on polymeric ionic liquid-based monolith (PILM) as extractive medium was used to concentrate these three organic acid preservatives. Because hydrophobic and ion-exchange interactions co-contributed to the extraction, the PILM-SCSE exhibited a high extractive capability towards analytes. To obtain optimum extraction performance, several SCSE parameters were investigated and discussed, including desorption solvent, pH value, ionic strength in the sample matrix, and the extraction and desorption time. Under the optimized extraction conditions, limits of detection of 0.16, 1.08, and 0.18 ?g/L (S/N=3) and quantification limits of 0.52, 3.42, and 0.61 (S/N=10) were obtained for SA, BA, and CA, respectively. The method also showed good linearity and reproducibility, as well as advantages such as simplicity, low cost, and high feasibility. Finally, the proposed method was successfully applied to the determination of SA, BA, and CA in real juices and soft drinks, and the recoveries ranged from 63.0 to 107 %.
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The extent of the influence and flux estimation of volatile mercury from the aeration pool in a typical coal-fired power plant equipped with a seawater flue gas desulfurization system.
Sci. Total Environ.
PUBLISHED: 01-07-2013
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Before being discharged, the waste seawater from the flue gas desulfurization system of coal-fired power plants contains a large amount of mercury, and is treated in aeration pools. During this aeration process, part of the mercury enters the atmosphere, but only very limited impact studies concerning this have been carried out. Taking a typical Xiamen power plant as an example, the present study targeted the elemental mercury emitted from the aeration pool. Concentrations of dissolved gaseous mercury as high as 1.14 ± 0.17 ng·L(-1) were observed in the surface waste seawater in the aeration pool, and gaseous elemental mercury (GEM) as high as 10.94 ± 1.89 ng·m(-3) was found in the air above the pool. To investigate the area affected by this GEM through air transfer, the total mercury in the dust and topsoil samples around the aeration pool were analyzed. Much higher values were found compared to those at a reference site. Environmental factors other than solar radiation had limited influence on the concentrations of the mercury species in the pool. A simulation device was built in our laboratory to study the flux of mercury from the aeration pool into the air. The results showed that more than 0.59 kg of mercury was released from the aeration pool every year, occupying 0.3% of the total mercury in the waste seawater. The transfer of mercury from water to air during the aeration pool and its environmental influence should not be ignored.
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Preparation of cation-exchange stir bar sorptive extraction based on monolithic material and its application to the analysis of soluble cations in milk by ion chromatography.
Analyst
PUBLISHED: 08-31-2011
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In this study, a new cation-exchange coating for stir bar sorptive extraction (SBSE) based on poly (acrylic acid-ethylene dimethacrylate) monolithic material was synthesized. The effect of polymerization conditions such as the ratio of functional monomer to cross-linker and the content of porogenic solvent on the extraction efficiencies were investigated in detail. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to evaluate the usability of the new coating for the extraction of inorganic cations, the analysis of soluble K(+), Mg(2+) and Ca(2+) in milk by ion chromatography with conductivity detection was selected as a paradigm. Several extractive parameters, including pH value in sample matrix, desorption solvent, extraction and desorption time were optimized. Under the optimum conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target cations were achieved within the range of 0.12-0.28 and 0.4-0.92 ?g L(-1), respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction of inorganic cations. Finally, the proposed method was successfully used to analyse three different trademarks of commercial milk samples with satisfactory recoveries in the range of 71.1% to 102.8%.
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[Advance of stir bar sorptive extraction].
Se Pu
PUBLISHED: 08-19-2011
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Stir bar sorptive extraction (SBSE) is an environmentally-friendly technology of sample preparation which combines extraction, cleanup and enrichment together, and it has been developed rapidly and widely applied to the trace enrichment of various target analytes in environmental, food and biological samples. Based on our research, the advance of SBSE, especially, the development of new coatings, are reviewed. At the same time, the possible development orientations of SBSE are discussed.
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Preparation, characterization and application of a new stir bar sorptive extraction based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith.
J Sep Sci
PUBLISHED: 08-01-2011
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In this study, a new stir bar sorptive extraction (SBSE) coating based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) was prepared. The influences of the contents of monomer in polymerization mixture and the percentage of porogen solvent on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy, were used to characterize the monolithic material. The analysis of oxfendazole (OFZ) and mebendazole (MBZ) in milk and honey samples by the combination of SBSE with HPLC with diode array detection was selected as paradigms for the practical evaluation of the new coating. Under the optimized extraction conditions, the limits of detection (S/N=3) for OFZ and MBZ were 0.23-0.60 ?g/L in milk and 0.24-1.08 ?g/L in honey, respectively. The method also showed good linearity, repeatability, high feasibility and acceptable recoveries for real samples. At the same time, the extraction performance and the distribution coefficients (K(VPMB/W)) of OFZ and MBZ on SBSE-VPMB were compared with other SBSEs based on porous monoliths and commercial SBSE.
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Determination of endocrine-disrupting compounds in water by carbon nanotubes solid-phase microextraction fiber coupled online with high performance liquid chromatography.
Talanta
PUBLISHED: 04-15-2011
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The commercial solid phase microextraction (SPME) fibers are not stable enough in organic solvent and tend to swell and strip off from the silica fiber in the high performance liquid chromatography (HPLC) mobile phase, and therefore the application of SPME coupled online with HPLC is limited. In this study, an SPME fiber coated with single walled carbon nanotubes (SWCNTs), prepared by means of electrophoretic deposition, was coupled on line to HPLC for the determination of four endocrine-disrupting compounds, i.e. bisphenol A (BPA), estrone (E(1)), 17?-ethynylestradiol (EE(2)) and octylphenol (OP), in aqueous samples. The results showed that the SWCNTs coating on the prepared fiber did not swell and strip off from the platinum fiber throughout the experiment, thus indicating a high resistance to the HPLC mobile phase, the mixture of water and acetonitrile. The SWCNTs fiber had similar (for OP) or higher (for BPA, EE(2) and E(1)) extraction efficiencies than the commonly used polyacrylate fiber, and had a lifetime of more than 120 operation times. Under the optimized conditions, the linearity of the proposed method was 1.0-30.0 ?g/L for BPA and OP and 3.0-90.0 ?g/L for E(1) and EE(2). The limits of detection (LODs; S/N=3) and limits of quantification (LOQs; S/N=10) of the method were 0.32-0.52 ?g/L and 1.06-1.72 ?g/L, respectively. Repeatability for one fiber (n=3) was in the range of 1.3-7.1% and fiber-to-fiber reproducibility (n=3) was in the range of 1.6-8.4%. The proposed method was successfully applied for the analysis of spiked tap water and seawater samples with recoveries from 81.8 to 97.3%.
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Novel extraction approach for liquid samples: Stir cake sorptive extraction using monolith.
J Sep Sci
PUBLISHED: 03-29-2011
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In this study, a new extraction approach for liquid samples - stir cake sorptive extraction using monoliths as extractive medium was developed. The preparation procedure of stir cake is very simple. First, monolithic cake is synthesized according to the in situ polymerization of monolith; then, the cake is inserted in an original unit (holder), which is constructed from a syringe cartridge and allows the magnetic stirring of the cake during the extraction process. The effects of dimension of monolithic cake and unit design on the extraction performance were optimized in detail. To demonstrate the usability of this new extraction approach, poly(vinylimidazole-divinylbenzene) was prepared and acted as the extractive cake. The analysis of steroid hormones in milk samples by the combination of stir cake with high-performance liquid chromatography with diode array detection, was selected as a paradigm for the practical evaluation of stir cake sorptive extraction. Under the optimized extraction conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target analytes were achieved within the range between 0.33-0.69 and 1.08-2.28??g/L, respectively. The method also showed good linearity, repeatability, high feasibility and acceptable recoveries. Because the monolithic cake does not contact with the vessel wall during stirring, there is no friction loss of extractive medium and the stir cake can be used for more than 1000?h.
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Mercury distribution in seawater discharged from a coal-fired power plant equipped with a seawater flue gas desulfurization system.
Environ Sci Pollut Res Int
PUBLISHED: 03-07-2011
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More and more coal-fired power plants equipped with seawater flue gas desulfurization systems have been built in coastal areas. They release large amount of mercury (Hg)-containing waste seawater into the adjacent seas. However, very limited impact studies have been carried out. Our research targeted the distribution of Hg in the seawater, sediment, biota, and atmosphere, and its environmental transportation.
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Electrosorption-enhanced solid-phase microextraction of trace anions using a platinum plate coated with single-walled carbon nanotubes.
Talanta
PUBLISHED: 03-02-2011
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A platinum plate coated with single-walled carbon nanotubes (SWCNTs@Pt) was prepared by means of electrophoretic deposition. Using the SWCNTs@Pt plate, an electrosorption-enhanced solid-phase microextraction (EE-SPME) technique was proposed for the extraction of trace anions in water, described as follows: a positive potential was applied to the SWCNTs@Pt plate to extract F(-), Cl(-), Br(-), NO(3)(-) and SO(4)(2-) from water using electrosorption, and then a negative potential was applied to the plate placed in ultra-pure water for the desorption of the absorbed anions, and finally the desorbed anions were analyzed using ion chromatography (IC). The EE-SPME parameters, including extraction potential and time as well as desorption potential and time, were investigated. An analytical method based on the above procedures, i.e., EE-SPME-IC, was established and used for the analysis of trace anions in water. The results showed that the application of potential on the SWCNTs@Pt plate significantly enhanced the ion extraction efficiency, and an enrichment factor of 15-38 was achieved. The SWCNTs@Pt plate could be used more than 50 times without significant decay. The linear range, the limit of detection (S/N=3), the limit of quantification (S/N=10) and repeatability (n=7) of our EE-SPME-IC method were 1.0-150.0 ?g/L, 0.06-0.26 ?g/L, 0.19-0.85 ?g/L and 2.1-8.0%, respectively. The proposed method was successfully applied for the analysis of trace anions in deionized water, and acceptable recoveries between 65.3 and 121.1% were obtained for the spiked deionized water samples.
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Relationship of photosynthetic carbon fixation with environmental changes in the Jiulong River estuary of the South China Sea, with special reference to the effects of solar UV radiation.
Mar. Pollut. Bull.
PUBLISHED: 02-23-2011
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Phytoplankton cells in estuary waters usually experience drastic changes in chemical and physical environments due to mixing of fresh and seawaters. In order to see their photosynthetic performance in such dynamic waters, we measured the photosynthetic carbon fixation by natural phytoplankton assemblages in the Jiulong River estuary of the South China Sea during April 24-26 and July 24-26 of 2008, and investigated its relationship with environmental changes in the presence or the absence of UV radiation. Phytoplankton biomass (Chl a) decreased sharply from the river-mouth to seawards (17.3-2.1 ?g L(-1)), with the dominant species changed from chlorophytes to diatoms. The photosynthetic rate based on Chl a at noon time under PAR-alone increased from 1.9 ?g C (?g Chl a)(-1) L(-1) in low salinity zone (SSS<10) to 12.4 ?g C (?g Chl a)(-1) L(-1) in turbidity front (SSS within 10-20), and then decreased to 2.1 ?g C (?g Chl a)(-1) L(-1) in mixohaline zone (SSS>20); accordingly, the carbon fixation per volume of seawater increased from 12.8 to 149 ?g C L(-1) h(-1), and decreased to 14.3 ?g C L(-1) h(-1). Solar UVR caused the inhibition of carbon fixation in surface water of all the investigated zones, by 39% in turbidity area and 7-10% in freshwater or mixohaline zones. In the turbidity zone, higher availability of CO2 could have enhanced the photosynthetic performance; while osmotic stress might be responsible for the higher sensitivity of phytoplankton assemblages to solar UV radiation.
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An automatic gas-phase molecular absorption spectrometric system using a UV-LED photodiode based detector for determination of nitrite and total nitrate.
Talanta
PUBLISHED: 01-10-2011
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An automatic gas-phase molecular absorption spectrometric (GPMAS) system was developed and applied to determine nitrite and total nitrate in water samples. The GPMAS system was coupled with a UV-light emitting diode photodiode (UV-LED-PD) based photometric detector, including a 255 nm UV-LED as the light source, a polyvinyl chloride (PVC) tube of 14 cm as the gas flow cell, and an integrated photodiode amplifier to measure the transmitted light intensity. The UV-LED-PD detector was compact, robust, simple and of low heat production, comparing with detectors used in other GPMAS works. For nitrite measurement, citric acid was used to acidify the sample, and ethanol to catalyze the quantitative formation of NO(2). The produced NO(2) was purged with air flow into the UV-LED-PD detector, and the gaseous absorbance value was measured. The total nitrate could be determined after being reduced to nitrite with a cadmium column. Limits of detection for nitrite and nitrate were 7 ?mol/L and 12 ?mol/L, respectively; and linear ranges of 0.021-5 mmol/L for nitrite and 0.036-4 mmol/L for nitrate were obtained. Related standard deviations were 1.81% and 1.08% for nitrite and nitrate, respectively, both at 2 mmol/L. The proposed method has been applied to determine nitrite and total nitrate in some environmental water samples.
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Simple and sensitive determination of nitroimidazole residues in honey using stir bar sorptive extraction with mixed mode monolith followed by liquid chromatography.
J Sep Sci
PUBLISHED: 01-06-2011
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In the present study, we developed a simple and sensitive method for the simultaneous determination of metronidazole (MTZ), ronidazole (RNZ), dimetridazole (DMZ), and tinidazole (TNZ) in honey. Honey samples were diluted with water, then directly treated by stir bar sorptive extraction (SBSE) based on poly(methacrylic acid-3-sulfopropyl ester potassium salt-co-divinylbenzene) monolithic material. The analytes were analyzed by HPLC equipped with diode array detector. In the optimized process, several parameters, including the composition of desorption solvent, pH value and ionic strength in sample matrix, extraction, and desorption time, were investigated in detail. Under the optimized conditions, the detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target compounds were achieved within the range of 0.47-1.52 and 1.54-5.0??g/kg from spiked honey sample, respectively. The calibration curves showed the linearity ranging from 2 to 200??g/kg for dimetridazole and tinidazole, 5-200??g/kg for metronidazole and ronidazole. Method repeatability presented as intra- and interday precisions were found with the RSDs <4.43 and 4.41%, respectively. Finally, the developed method was successfully applied to the determination of nitroimidazoles in different honey samples and satisfactory recoveries of spiked target compounds were in the range of 71.1-114%.
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[Determination of bisphenol A in environmental water samples by stir bar sorptive extraction based on molecularly imprinted polymer].
Se Pu
PUBLISHED: 09-04-2010
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A new stir bar sorptive extraction (SBSE) based on molecularly imprinted polymer (MIP) with bisphenol A as template was prepared. Based on it, a simple, selective and sensitive method for the determination of bisphenol A (BPA) was developed combined with high performance liquid chromatography (HPLC) with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, the nature of desorption solvent, pH value and contents of inorganic salt in the sample matrix, were investigated. The optimized parameters for the extraction of BPA from water matrix with the MIP-SBSE are as follows: extraction and desorption time were 120 min and 10 min, respectively; the pH value of matrix was 10.0; using acetonitrile (including 1% acetic acid) as desorption solvent; no salt was added in the matrix. Under the optimized experimental conditions, the method showed good linearity between 1.0-200 microg/L. The detection limit (S/N = 3) and quantification limit (S/N = 10) of the proposed method for the BPA was 0.28 microg/L and 0.94 microg/L, respectively. The proposed method was successfully applied to the determination of the target compound in water samples. The recoveries of spiked target compound in real samples ranged from 96.0%-108.7%. The results indicated that the developed method possessed the advantages such as high sensitivity, simplicity, low cost and environmental friendliness.
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Mercury species in seawater and sediment of Xiamen western sea area adjacent to a coal-fired power plant.
Water Environ. Res.
PUBLISHED: 05-04-2010
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The purpose of this study was to investigate the concentrations and spatial distributions of mercury (Hg) species in seawater (including dissolved, particle, and total Hg) and sediment (including total and methyl Hg) of the Xiamen western sea area adjacent to a coal-fired power plant. The influence of the wastewater discharged from the seawater desulphurization (De-SO2) system of the power plant is discussed. Concentration of the three species of mercury in seawater from 18 sampling sites varied: dissolved ranged from 0.70 to 4.65 ng/L (mean 1.47 ng/L; median 1.12 ng/L); particulate ranged from not detected to 90.52 ng/L (mean 10.47 ng/L; median 1.26 ng/L); and total was 1.51 to 92.88 ng/L (mean 11.94 ng/L; median 2.84 ng/L). High concentrations of total Hg and particulate Hg, more than 70 ng/L, were observed in the area adjacent to the outfalls of the power plant. The Hg from the waste seawater of the power plant might be re-emitted to the atmosphere because it exists in seawater mainly in particulate attached form. The sediment total Hg concentrations ranged from 0.055 to 0.201 microg/g, with a mean of 0.126 microg/g and a median of 0.125 microg/g. Low methyl Hg concentrations in the sediment were observed in the study area, ranging from 0.017 to 0.256 ng/g as Hg, with a mean of 0.087 ng/g and a median of 0.081 ng/g. The ratios of methyl Hg to total Hg in the sediment were low, with a mean and median of 0.069%. Both total and methyl Hg were significantly linked to the sediment organic carbon (SOC).
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A new anionic exchange stir bar sorptive extraction coating based on monolithic material for the extraction of inorganic anion.
J Chromatogr A
PUBLISHED: 04-13-2010
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A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2-(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br-, NO3-, PO4(3-) and SO4(2-) were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.92-2.62 and 3.03-9.25 microg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0-92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions.
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Evaluation of the solid-phase microextraction fiber coated with single walled carbon nanotubes for the determination of benzene, toluene, ethylbenzene, xylenes in aqueous samples.
J Chromatogr A
PUBLISHED: 01-29-2010
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A solid-phase microextraction (SPME) fiber coated with single walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition and treated at 500 degrees C in H(2) stream. In order to evaluate the characteristics of the obtained fiber, it was applied in the headspace solid-phase microextraction (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample and quantification by gas chromatography with flame ionization detection (GC-FID). The results indicated that the thermal treatment with H(2) enhanced the extraction of the SWCNTs fiber for BTEX significantly. Thermal stability and durability of the fiber were also investigated, showing excellent stability up to 350 degrees C and life time over 120 times. In the comparison with the commercial CAR-PDMS fiber, the SWCNTs fiber showed similar and higher extraction efficiencies for BTEX. Under the optimized conditions, the linearity, LODs (S/N=3) and LOQs (S/N=10) of the method based on the SWCNTs fiber were 0.5-50.0, 0.005-0.026 and 0.017-0.088 microg/L, respectively. Repeatability for one fiber (n=3) was in the range of 1.5-5.6% and fiber-to-fiber reproducibility (n=3) was in the range of 4.2-8.3%. The proposed method was successfully applied in the analysis of BTEX compounds in seawater, tap water and wastewater from a paint plant.
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Distribution characteristics of total mercury and methylmercury in the topsoil and dust of Xiamen, China.
J Environ Sci (China)
PUBLISHED: 12-17-2009
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The levels and distribution of mercury (Hg) species, including total mercury (THg) and methylmercury (MeHg) in the topsoil and dust collected from twenty sampling stations located in different land function areas of Xiamen, China, were investigated. The THg concentrations in topsoil ranged from 0.071 to 1.2 mg/kg, and in dust ranged from of 0.034 to 1.4 mg/kg. For stations where the THg of dust was less than 0.31 mg/kg, THg concentrations in the topsoil were significantly correlated to those in the corresponding dust (r = 0.597, n = 16, P = 0.014). The MeHg concentrations in topsoil were varied between 0.14 and 5.7 microg/kg. The ratios of MeHg/THg in the topsoil ranged from 0.069% to 0.74%. The range of MeHg concentration in the dust were 0.092-2.3 microg/kg. The ratios of MeHg/THg in the dust were at the same level as those in the topsoil. The MeHg concentrations in both topsoil and dust were linked to corresponding THg concentrations and soil organic matter. Neither THg nor MeHg concentration in the topsoil and dust was obviously linked to the land function.
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On-line solid-phase extraction coupled with liquid chromatography/electrospray ionization mass spectrometry for the determination of trace tributyltin and triphenyltin in water samples.
Rapid Commun. Mass Spectrom.
PUBLISHED: 11-12-2009
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On-line solid-phase extraction (SPE) for pre-concentration and sample cleanup is one strategy to reduce matrix effects and to simultaneously improve detection sensitivity in liquid chromatography/mass spectrometry (LC/MS). This paper describes an on-line SPE-LC/MS method for the determination of tributyltin (TBT) and triphenyltin (TPhT) at trace levels in water samples. The direct coupling of an on-line C18 pre-column to LC/MS was used to pre-concentrate TBT and TPhT at trace levels from waters and to remove interfering matrix effects. Pre-concentration was followed by separation of TBT and TPhT on a C18 column using a mobile phase containing 0.1% (v/v) HCOOH/5 mM HCOONH4 and methanol. While both electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) can be interfaced with MS for the detection of TBT and TPhT, ESI-MS was preferred for this application. The calibration curve for the targets was linear in the concentration range 0.1-30 microg L(-1). The detection limit (signal-to-noise (S/N) ratio = 3) was 0.02 microg L(-1) when 3.0 mL of sample was enriched on the C18 pre-column. The recoveries of TBT and TPhT in spiked waters were from 81.0 to 101.9%. The reproducibilities for the analysis of the standard mixture (10 microg L(-1)) for TBT and TPhT were 13.1 and 5.0%, respectively. The developed method was an easy and fast way to analyze TBT and TPhT in water samples.
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Preparation of a mixed stir bar for sorptive extraction based on monolithic material for the extraction of quinolones from wastewater.
J Chromatogr A
PUBLISHED: 08-12-2009
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In this study, a novel mixed mode monolithic material was prepared and acted as the SBSE coating. The monolithic material was prepared by in situ copolymerization of methacrylic acid-3-sulfopropyl ester potassium salt (MASE) and divinylbenzene (DB) in the presence of a porogen solvent containing cyclohexanol, 1-dodecanol, and water with azobisisobutyronitrile as initiator. The influences of the contents of the porogen solvent and monomer in the polymerization mixture on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy and infrared spectroscopy were used to characterize the monolithic material. To achieve optimum extraction performance for quinolones, several parameters, including pH value, desorption solvent, ionic strength in sample matrix, extraction and desorption time were investigated. The results show that under the optimized experimental conditions, the method has good sensitivity, linearity, simplicity and low cost. The extraction performance of present method to the target compounds was compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSEs which based on monolithic materials. The comparative results indicate that present SBSE can extract the analytes more effectively than other SBSEs because both ion-exchange and hydrophobic interactions contribute to the extraction of quinolones.
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[Simultaneous determination of tetracycline and quinolone antibiotics in environmental water samples using solid phase extraction-ultra pressure liquid chromatography coupled with tandem mass spectrometry].
Se Pu
PUBLISHED: 05-20-2009
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Using HLB cartridge for extraction and cleanup, a method for simultaneous determination of 4 tetracycline and 6 quinolone antibiotics in environmental water samples was developed by ultra pressure liquid chromatography coupled with tandem mass spectrometry. Using river water and sea water as matrices and carbadox as surrogate, the recoveries and relative standard deviations (RSD, n = 4) were 94.0% - 117.0% and 2.0% - 9.7% for 4 tetracyclines at 20.0 ng/L and 100.0 ng/L spiking levels and 63.6% - 93.9% and 1.6% - 8.1% for 6 quinolones at 5.0 ng/L and 20.0 ng/L spiking levels, respectively. The detection limits were 20.0 ng/L for 4 tetracyclines and 0.4 ng/L for 6 quinolones. The method has been successfully applied to the survey of 10 target antibiotic residues in Jiulong River estuary, Fujian.
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Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis.
J Chromatogr A
PUBLISHED: 05-02-2009
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In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%.
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Development and validation of stir bar sorptive extraction of polar phenols in water followed by HPLC separation in poly(vinylpyrrolididone-divinylbenzene) monolith.
J Sep Sci
PUBLISHED: 04-11-2009
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An effective and simple method for polar phenols in water matrix was developed by using stir bar sorptive extraction (SBSE) based on a hydrophilic poly(vinylpyrrolididone-divinylbenzene) (VPDB) monolithic material and HPLC analysis. To achieve optimum extraction performance for phenols, several parameters, including extraction and desorption time, desorption solvent, pH value, and ionic strength of sample matrix, were investigated. Under the optimized experimental conditions, eight phenols were directly enriched from water samples and analyzed by HPLC-DAD. The detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.72-1.37 and 2.40-4.27 ng/mL from spiked water, respectively. Recoveries of eight phenolic compounds were found in the range of 55.2-95.9%. The calibration curves showed the linearity ranging from 5 to 150 ng/mL with linear regression coefficient R(2) values above 0.98. Method repeatability presented as intra- and interday precisions were also found with the RSDs less than 4.10 and 7.61%, respectively. The distribution coefficients between VPDB and water (K(VPDB/W)) for phenolic compounds were also calculated and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the target compounds in tap water, sea water and wastewater samples.
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[Determination of sulfite in flue gas desulfurization with seawater by ion chromatography].
Se Pu
PUBLISHED: 03-02-2009
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The technology for flue gas desulfurization (FGD) with seawater is widely adopted by coal-fired power plants in coastal areas. SO2 in the flue gas is absorbed by alkaline seawater and transfered in aqueous phase as sulfite (SO3(2-)), and most SO3(2-) is transformed to sulfate (SO4(2-)) after an aeration process. The remaining SO3(2-) in the seawater discharged to sea area may be harmful to marine organism because of its biological toxicity, thus it is necessary to determine the concentration of SO3(2-) in the seawater for desulfurization. In this study, the method of determination of SO3(2-) in the seawater by ion chromatography was investigated. The separation was achieved on an IonPac AS14A column with 14 mmol/L NaOH-12 mmol/L Na2 CO3 solution as the mobile phase at a flow rate of 1.2 mL/min, and the detection was performed by a pulsed amperometric detector. Formaldehyde was added as a protective agent when sampling because the SO3(2-) is easy to be oxidized. To avoid the formation of Mg (OH)2 in the mobile phase with high pH value which might block the column, the Mg(2+) in seawater was precipitated by NaOH solution (pH 12.0) before sample determination. The method showed good linearity within the range of 0-100 mg/L with an average recovery of 116.8%. The method detection limit (MDL) reached as low as 0.05 mg/L. The relative standard deviations (RSD) for seawater matrix samples spiked at levels of 7.5, 25.0 and 75.0 mg/L were 2.1% 3.1% and 4.0% (n = 9) , respectively. The method has been applied for the determination of SO3(2-) in flue gas desulfurization seawater with the advantages of being fast, sensitive and selective.
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Assessment of the bioaccessibility of polycyclic aromatic hydrocarbons in topsoils from different urban functional areas using an in vitro gastrointestinal test.
Environ Monit Assess
PUBLISHED: 01-31-2009
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Profiles of the bioaccessibility of soil polycyclic aromatic hydrocarbons (PAHs) in different urban functional areas of Xiamen City, Fujian, China were investigated. A physiologically based in vitro test was used to evaluate the bioaccessibility of total and individual PAHs. There was no obvious correlation between total concentrations of PAHs and bioaccessibility during the gastrointestinal phase for the soils from different functional areas. Results showed that the bioaccessibility variation in the gastrointestinal phase (ranging from 14.6% to 63.2%) was significantly higher than that in the gastric phase (ranging from 4.9% to 21.8%). The bioaccessibility in the gastrointestinal phase was not only determined by soil organic materials but also directly related to physical and chemical properties of individual PAHs, except for two-ring PAHs. Increasing soil organic material content or decreasing ring numbers of PAHs could result in the decrease of PAH bioaccessibility. The total PAH bioaccessibility was largely contributed by individual PAHs with relatively high molecular weight.
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Reverse flow injection analysis of nanomolar soluble reactive phosphorus in seawater with a long path length liquid waveguide capillary cell and spectrophotometric detection.
Talanta
PUBLISHED: 01-29-2009
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A novel reverse flow injection analysis method coupled with a liquid waveguide capillary cell (LWCC) and spectrophotometric detection for the determination of nanomolar soluble reactive phosphorus in seawater was established. Reagent was injected into the sample stream and detected in a 2-m path length LWCC with detection wavelength set at 710 nm. Experimental parameters, including the reagent concentration, the injection volume, the flow rate and the length of the mixing coil, were optimized based on univariate experimental design. The interference of silicate and arsenate were also investigated. Under optimized conditions, the linearity and the detection limit of the proposed method were found to be 0-165.0 nM and 0.5 nM, which was estimated to be three times the standard deviation of the measurement blanks (n=9). The relative standard deviations for the determination of 24.7 and 82.5 nM samples were 1.54% and 1.86% (n=9), respectively. Three seawater samples were analyzed with recoveries ranging from 87.8% to 101.8%. Using the Students t-test at the 95% confidence level, the results of the proposed method and a segmented flow analyzer reference method for determination of the two samples showed no significant difference. The proposed method had the advantages of being less reagent consuming, more sensitive and with higher throughput (15 h(-1)).
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A novel stir bar sorptive extraction coating based on monolithic material for apolar, polar organic compounds and heavy metal ions.
Talanta
PUBLISHED: 01-29-2009
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In this study, a novel stir bar sorptive extraction (SBSE) based on monolithic material (SBSEM) was prepared. The monolithic material was obtained by in situ copolymerization of vinylpyrrolidone and divinylbenzene in the presence of a porogen solvent containing cyclohexanol and 1-dodecanol with azobisisobutyronitrile as initiator. The influences of polymerization conditions on the extraction efficiencies were investigated, using phenol and p-nitrophenol as detected solutes. The monolithic material was characterized by various techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, infrared spectroscopy. Polycyclic aromatic hydrocarbons were used to investigate the extraction efficiencies of SBSEM for apolar analytes. Hormones, aromatic amines and phenols were selected as test analytes to investigate the extraction efficiencies of SBSEM for weakly and strongly polar compounds. The results showed that the new SBSEM could enrich the above-mentioned organic compounds effectively. It is worthy to mention that the SBSEM can enrich some heavy metal ions, such as Cu(2+), Pb(2+), Cr(3+) and Cd(2+), through coordination adsorption. To our best knowledge, that is the first to use SBSE to enrich heavy metal ions.
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Solid-phase extraction of polar organophosphorous pesticides from aqueous samples with oxidized carbon nanotubes.
J Environ Monit
PUBLISHED: 01-27-2009
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The development of new sorbents, which are able to trap polar compounds, is a growing research field in solid-phase extraction (SPE). In this study, multi-walled carbon nanotubes (MWCNTs) and single-walled carbon nanotubes (SWCNTs) were oxidized in air at 600 degrees C and 500 degrees C, respectively, for 2 h. MWCNTs, SWCNTs, air oxidized MWCNTs (OMWCNTs) and SWCNTs (OSWCNTs) (200 mg of each) were packed in SPE cartridges. The four cartridges obtained, together with a commercial Oasis HLB cartridge, were used to extract six polar organophosphorous pesticides (OPPs), i.e., dichlorvos, methamidophos, acephate, omethoate, monocrotophos and dimethoate, from an aqueous sample. The results showed that the oxidation process significantly enhanced the adsorption abilities of both SWCNTs and MWCNTs for polar OPPs. A comparative study indicated that OSWCNTs were more effective than Oasis HLB for the extraction of methamidophos and acephate and as effective as Oasis HLB for the other four OPPs from aqueous samples. When 100 mL of a natural sample was spiked with OPPs and extracted with OSWCNTs, the recoveries of five of the six polar OPPs (methamidophos excepted) ranged from 79.1 to 101.9%. The detection limits of the method based on OSWCNTs was found to be 0.07-0.12 microg L(-1).
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Simple and sensitive monitoring of sulfonamide veterinary residues in milk by stir bar sorptive extraction based on monolithic material and high performance liquid chromatography analysis.
J Chromatogr A
PUBLISHED: 01-11-2009
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A simple, rapid, and sensitive method for the quantitative monitoring of five sulfonamide antibacterial residues (SAs) in milk was developed by stir bar sorptive extraction (SBSE) coupling to high performance liquid chromatography with diode array detection. The analytes were concentrated by SBSE based on poly (vinylimidazole-divinylbenzene) monolithic material as coating. The extraction procedure was very simple, milk was diluted with water then directly sorptive extraction without elimination of fats and protein in samples was required. To achieve optimum extraction performance for SAs, several parameters, including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. Under the optimized experimental conditions, low detection limits (S/N=3) quantification limits (S/N=10) of the proposed method for the target compounds were achieved within the range of 1.30-7.90 ng/mL and 4.29-26.3 ng/mL from spiked milk, respectively. Good linearities were obtained for SAs with the correlation coefficients (R(2)) above 0.996. Finally, the proposed method was successfully applied to the determination of SAs compounds in different milk samples and satisfied recoveries of spiked target compounds in real samples were obtained.
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Preparation of solid-phase microextraction fiber coated with single-walled carbon nanotubes by electrophoretic deposition and its application in extracting phenols from aqueous samples.
J Chromatogr A
PUBLISHED: 01-06-2009
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A novel solid-phase microextraction (SPME) Pt fiber coated with single-walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition (EPD) and applied to the determination of phenols in aqueous samples by direct immersion (DI)-SPME-HPLC-UV. The results revealed that EPD was a simple and reproducible technique for the preparation of SPME fibers coated with SWCNTs without the use of adhesive. The obtained SWCNT coating did not swell in organic solvents nor strip off from substrate, and possessed high mechanical strength due to the strong Van der Waals attractions between the surfaces of the SWCNTs. The prepared SPME fiber was conductive since both SWCNT coating and Pt wire were conductive. Using Pt wire as substrate, the fiber was unbreakable. Owing to the presence of oxygenated groups on SWCNTs and the high surface area of SWCNTs, the SWCNT fiber was similar to or superior to commercial PA fiber in extracting the studied phenols from aqueous sample. A durability of more than 80 analyses was achieved for one unique fiber. Under optimized conditions, the detection limits for the phenols varied between 0.9 and 3.8 ng/mL, the precisions were in the range of 0.7-3.2% (n=3), and linear ranges were within 10 and 300 ng/mL. The method was successfully applied to the analysis of spiked seawater and tap water samples with the recoveries from 87.5 to 102.0%.
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Sensitive determination of strongly polar aromatic amines in water samples by stir bar sorptive extraction based on poly(vinylimidazole-divinylbenzene) monolithic material and liquid chromatographic analysis.
J Chromatogr A
PUBLISHED: 01-05-2009
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A simple and sensitive method for the determination of polar aromatic amines (PAAs) was developed using stir bar sorptive extraction (SBSE) coupling to high-performance liquid chromatography. A hydrophilic poly(vinylimidazole-divinylbenzene) (VIDB) monolithic material was prepared and acted as SBSE coating. The influences of polymerization conditions for VIDB on the extraction efficiency were investigated using aniline and 2,4-dinitroaniline as detected solutes. To achieve optimum extraction performance for PAAs, several parameters including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. The results showed that under the optimized experimental conditions, the method showed good sensitivity and excellent recoveries, as well as advantages such as linearity, simplicity, low cost and high feasibility. The extraction performance of present method to the target compounds also compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSE which based on monolithic materials. Finally, the proposed method was successfully applied to the determination of PAAs in lake and sea waters, and excellent recoveries of spiked target compounds in real samples were obtained.
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Preparation of a stir bar sorptive extraction coating based on molecularly imprinted polymer and its application in the extraction of dienestrol and hexestrol in complicated samples.
Se Pu
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A new stir bar sorptive extraction (SBSE) coating based on molecularly imprinted polymer (MIP) with diethylstilbestrol as replaced template molecule was prepared. The influences of the contents of template molecule and monomer in the polymerization mixture on the extraction performance of MIP-SBSE were investigated thoroughly. The MIP was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to evaluate the usability of the new coating, the MIP-SBSE was combined with high performance liquid chromatography (HPLC) and diode array detector (DAD) with dienestrol (DS) and hexestrol (HS) as detected solutes. To achieve optimally selective extraction performance for DS and HS, several parameters, including extraction and desorption times, desorption solvent, ionic strength and pH value in sample matrix were investigated. The results showed that under the optimized experimental conditions, the present method has high selectivity and sensitivity. When drying-redissolving procedure was taken during sample preparation, the limits of detection for DS and HS were as low as 0.04 microg/L and 0.14 micorg/L, respectively. Good linearities were obtained for analytes with the correlation coefficients (R2) above 0.99. Finally, the proposed method was successfully applied to the determination of DS and HS in wastewater, honey and cow urine samples. The recoveries of spiked target compounds in real samples ranged from 61.3% to 120%. The developed method is simple, selective, sensitive and applicable for the analysis of trace DS and HS in complicated samples.
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New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC.
Anal Bioanal Chem
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A novel porous monolith has been prepared and used as a sorbent in stir-cake-sorptive extraction (SCSE). The monolithic material was prepared by in-situ copolymerization of allyl thiourea (AT) and divinylbenzene (DB) in the presence of dimethylformamide as a porogen solvent. To optimize the polymerization conditions, different monoliths with different ratios of functional monomer to porogenic solvent were prepared, and their extraction efficiency was investigated in detail. The monolith was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, and infrared spectroscopy. Analysis of polar phenols in environmental water samples by a combination of ATDB-SCSE and HPLC with diode-array detection was selected as a model for the practical application of the new sorbent. Several extraction conditions, including extraction and desorption time, pH, and ionic strength of the sample matrix were optimized. The results showed that the new monolith had high affinity for polar phenols and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the phenols, within the ranges 0.18-0.90 and 0.59-2.97 ?g L(-1), respectively. The linearity of the method was good, and the method enabled simple, practical, and low-cost extraction of these analytes. The distribution coefficients between ATDB and water (K(ATDB/W)) were calculated for the phenolic compounds and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the compounds in three environmental water samples, with acceptable recovery and satisfactory repeatability.
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Preparation of a new polymeric ionic liquid-based monolith for stir cake sorptive extraction and its application in the extraction of inorganic anions.
J Chromatogr A
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In this study, a novel stir cake sorptive extraction (SCSE) sorbent based on polymeric ionic liquid-based monolith (PILM) for the extraction of inorganic anions was prepared. In the presence of a porogen solvent containing 1-propanol and dimethylformamid, an ionic liquid, 1-ally-3-methylimidazolium chloride was used as monomer to copolymerize in situ with ethylene dimethacrylate to form PILM. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detail. The PILM was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy. In order to investigate the extraction capacity of PILM-SCSE for inorganic anions, the SCSE was combined with ion chromatography with conductivity detection, F(-), Cl(-), NO(2)(-), Br(-), NO(3)(-), PO(4)(3-) and SO(4)(2-) were selected as detected solutes. Several extractive parameters, including pH values in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.11-2.08 and 0.37-6.88 ?g/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect different water samples include commercial purified water, tab water and river water. Acceptable recoveries and satisfactory repeatability were obtained. To the best of our knowledge, this is the first to use polymeric ionic liquid to enrich inorganic anions.
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[Simultaneous determination of 87 pesticides in river water and seawater using solid phase extraction-gas chromatography-mass spectrometry].
Se Pu
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A method for the simultaneous determination of 87 commonly used pesticides in China including 24 organophosphorous pesticides, 15 organochlorine pesticides, 12 azoles, 9 pyrethroids, 7 amides and anilines, 5 carbamates and other 15 pesticides in river water and seawater was established using solid phase extraction (SPE)-gas chromatography-mass spectrometry (GC-MS). GC-MS parameters influencing separation and sensitivity were optimized, and the effects of sample volume, pH and salinity on SPE were investigated. The purification was performed using NH2 SPE cartridge. An internal standard and 5 surrogates were used for data analysis and quality control. The results indicated that under the optimized conditions the limits of detection were in the range of 0.1 - 6.6 ng/L. For most target pesticides, recoveries were between 60% and 120% with relative standard deviations (RSDs, n = 4) of 0.01% - 9.7% at the spiked levels of 5 ng/L and 20 ng/L in real river water and sea water matrices. The method was successfully applied to monitor multi-class pesticides in surface water in Fujian Jiulong estuary, and 20 pesticides including 5 organophosphorous pesticides, 3 amides, 4 azoles, 3 carbamates, 2 pyrethroids and 3 other pesticides were detected in the mass concentration range of 1.18 - 660.93 ng/L. The proposed method can meet the requirement for the determination of trace pesticide residues in water samples.
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Reverse flow injection analysis method for catalytic spectrophotometric determination of iron in estuarine and coastal waters: a comparison with normal flow injection analysis.
Talanta
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A method for determining iron in seawater had been developed by coupling reverse flow injection analysis (rFIA) and catalytic spectrophotometric detection with N,N-dimethyl-p-phenylenediamine dihydrochloride (DPD). With a seawater sample or a standard solution as the carrier, the mixture of DPD and buffer was injected into the carrier stream quantitatively and discretely. After mixing with H(2)O(2), the DPD was oxidized to form two pink semiquinone derivatives that were monitored at 514 nm wavelength with a reference at 700 nm. The method detection limit was 0.40 nmol L(-1), lower than half of that of normal flow injection analysis (nFIA) method. The sample throughput was 10h(-1) with triplicate determination, compared with 4h(-1) for nFIA-DPD method. The analysis results of the certified seawaters CASS-4 (12.33 ± 0.18 nmol L(-1)) and NASS-5 (3.47 ± 0.23 nmol L(-1)) well agreed with the certified values (12.77 ± 1.04 and 3.71 ± 0.63 nmol L(-1), respectively). The typical precision of the method for a 2.97 nmol L(-1) iron sample was 4.49% (n=8). Interferences from copper and salinity were investigated. An instrument was assembled based on the proposed method and applied successfully to analyze total dissolvable iron (TDFe) in surface seawater samples collected from the Pearl River Estuary, the results of which revealed non-conservative behavior of TDFe during the estuarine mixing. Results for these samples with both rFIA-DPD and nFIA-DPD methods showed good agreement with each other. The proposed method was superior to the currently used nFIA-DPD method, particularly when it is adapted for field and in situ deployment, due to its lower reagent consumption, higher sample throughput and keeping the manifold tubing clean.
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