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A gas phase chemiluminescence (GPCL)-based method for trace measurement of arsenic has been recently described for the measurement of arsenic in water. The principle is based on the reduction of inorganic As to AsH(3) at a controlled pH (the choice of pH governs whether only As(III) or all inorganic As is converted) and the reaction of AsH(3) with O(3) to produce chemiluminescence (Idowu et al., Anal. Chem. 78 (2006) 7088-7097). The same general principle has also been used in postcolumn reaction detection of As, where As species are separated chromatographically, then converted into inorganic As by passing through a UV photochemical reactor followed by AsH(3) generation and CL reaction with ozone (Idowu and Dasgupta, Anal. Chem. 79 (2007) 9197-9204). In the present paper we describe the measurement of As in different soil and dust samples by serial extraction with water, citric acid, sulfuric acid and nitric acid. We also compare parallel measurements for total As by induction coupled plasma mass spectrometry (ICP-MS). As(V) was the only species found in our samples. Because of chloride interference of isobaric ArCl(+) ICP-MS analyses could only be carried out by standard addition; these results were highly correlated with direct GPCL and LC-GPCL results (r(2)=0.9935 and 1.0000, respectively). The limit of detection (LOD) in the extracts was 0.36 microg/L by direct GPCL compared to 0.1 microg/L by ICP-MS. In sulfuric acid-based extracts, the LC-GPCL method provided LODs inferior to those previously observed for water-based standards and were 2.6, 1.3, 6.7, and 6.4 microg/L for As(III), As(V), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA), respectively.
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PMID:Measurement of soil/dust arsenic by gas phase chemiluminescence. 1880 48

Several solvent mixtures and techniques for the extraction of arsenic (As) species from rice flour samples prior to their analysis by HPLC-ICP-MS were investigated. Microwave-assisted extraction using water at 80 degrees C for 30 min provided the highest extraction efficiency. Total recoveries of extracted As species were in good agreement with the total As concentrations determined by ICP-MS after microwave-assisted acid digestion of the samples. Arsenite [As(III)], arsenate [As(V)] and dimethylarsinic acid (DMAA) were the main species detected in rice flour samples.
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PMID:The extraction and speciation of arsenic in rice flour by HPLC-ICP-MS. 1880 56

An anion exchange HPLC-ICP-MS procedure allowing the simultaneous multielemental speciation analysis of arsenic, selenium, antimony and tellurium has been developed. Four arsenic species (As(III), As(V), monomethylarsonic acid and dimethylarsinic acid), two selenium species (Se(IV) and Se(VI)) may be determined in a single run as well as one antimony (Sb(V)) and one tellurium species (Te(VI)). Alternatively Sb and/or Te may be used as internal standards for As and Se speciation studies. Optimisation of ICP-MS conditions led to satisfactory relative (0.01 (Sb(V)) to 1.8 (Se(VI)) ng ml(-1)) and absolute detection limits (1-180 pg). Reproducibility ranged from 3.1 to 5.6% and the linearity was verified in the 0-200 ng ml(-1) range.
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PMID:Multielemental speciation of As, Se, Sb and Te by HPLC-ICP-MS. 1896 69

Performances of two atomic detectors, Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) and Atomic Fluorescence Spectrometry (AFS) have been compared for arsenic speciation in environmental samples. Instrumental couplings, based on the use of high performance liquid chromatography (HPLC), hydride generation (HG), and the two atomic detectors were used for the speciation of arsenite, arsenate, dimethylarsinic acid and monomethylarsonic acid. Optionally, arsenobetaine was also determined using on-line ultraviolet (UV) photooxidation. The detection limits ranging from 0.1 to 0.3 mug l(-1) (as As) and the precision >10% RSD obtained with HPLC-(UV)-HG-AFS were comparable with those obtained with HPLC-(UV)-HG-ICP-MS. Both instrumental coupling were applied to the NRCC-TORT-1 and several environmental samples, such as seawater, freshwater, sediments, bivalves and bird eggs, taken from two areas with different degrees of pollution. No influence of the sample matrix was observed on the results using external calibration and standard additions methods, for both coupled techniques.
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PMID:A comparison between ICP-MS and AFS detection for arsenic speciation in environmental samples. 1896 57

A microwave-assisted digestion procedure was developed in presence of concentrated nitric acid (2.0 ml) and 30% hydrogen peroxide (0.20 ml) using a closed pressurized microwave digestion system for the determination of total anionic and total cationic arsenic compounds reside in oyster tissue. At 450 W for 15 min digestion, 74% of anionic arsenic, and 31% of cationic arsenic (105% total arsenic) were retrieved. At 300 W microwave power, 68% of anionic and 30.5% of cationic arsenic (98.5% total arsenic), and 100 W, 63% of anionic and 31% of cationic arsenic (94% total arsenic) were extracted out. The methanol water mixture (9:1) was cull out, exclusively 31.6% of anionic and 29% of cationic arsenic compounds (60.6% total). The dimethylarsinoylriboside (phosphate-arsenosugar) was the predominant arsenic species, along with arsenobetaine (AB), dimethylarsinic acid (DMA), inorganic arsenic, methylarsonic acid (MA), arsenocholine (AC), trimethylarsineoxide (TMAO) and tetramethylarsonium ion (TMI). Some other arsenic compounds, those were not matched with the retention time of the available standards, were also detected. Arsenosugar was fragile and adequately transmuted to DMA (100%), AB and AC to TMAO (100%) when 450 W microwave power was applied for 15 min. The separation and quantification of arsenic compounds in the microwave digests and extracts, were carried out in anion (PRP-X100) and cation (LC-SCX) exchange columns using ICP-MS as arsenic specific detector. The procedure was also validated by determining the total cationic and total anionic arsenic compounds present in DORM 1.
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PMID:Determination of total cationic and total anionic arsenic species in oyster tissue using microwave-assisted extraction followed by HPLC-ICP-MS. 1896 61

A gradient anion exchange chromatographic technique was developed for the separation of arsenobetaine (AsB), arsenocholine (AsC), arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) in one chromatographic run. This technique used low residue ammonium carbonate buffer and the inductively coupled plasma-mass spectrometry (ICP-MS) chromatograms showed little baseline drift. Gradient elution improved peak shape and peak separation. The separation was completed in approximately 27 min with low detection limits (0.017-0.029 mug As kg(-1)). Baseline resolution of all the arsenic species evaluated was achieved when the concentration of AsC was less than approximately 12.5 mug As kg(-1). This technique was successfully applied to different extracts of a standard reference material, TORT-2, and lobster tissue. AsB was found to be the major arsenic species present. AsC, DMAA, MMAA and As(V) were also found, although MMAA was not detected in all of the TORT-2 extracts. Two unknown peaks found may be due to the presence of arsenosugars or other arsenic species. Discrepancy between extraction recoveries previously determined using flow injection-ICP-MS and the high-performance liquid chromatography-ICP-MS was observed in some cases. The differences may be due to the extraction technique and/or conditions at which the extractions were performed.
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PMID:A gradient anion exchange chromatographic method for the speciation of arsenic in lobster tissue extracts. 1896 40

The toxicity of certain elements is known to be related to their organic substituents and/or oxidation states. As such, total elemental determinations do not always yield sufficient information for accurate risk assessments and therefore speciation or fractionation data are required. In order to obtain fractionation data for trace levels of arsenic and selenium, a novel sequential pneumatic nebulisation (PN)/hydride generation (HG) inductively coupled plasma mass spectrometry (ICP-MS) method was developed. The method offers the advantage of sample introduction via either PN or HG by simply rotating a 4-way switching valve while the system is in operation. In PN mode, the liquid sample is aspirated into ICP, allowing for the determination of the total amount of each element, whilst in HG mode only the arsenic and selenium species that form volatile hydrides are determined. Conveniently, in the case of arsenic, this allows for differentiation between the four most toxic arsenic species (arsenate, arsenite, monomethylarsonic acid and dimethylarsinic acid), which form volatile hydrides, and the virtually non-toxic forms (arsenobetaine, arsenosugars, etc.), which do not. This allows for the rapid estimation of the amounts of toxic and non-toxic arsenic species present in a sample. For arsenic, the technique gave detection limits of 36 ng l(-1) in PN mode and 1 ng l(-1) in HG mode. For selenium, detection limits of 150 ng l(-1) were achieved in PN mode and 220 ng l(-1) in HG mode. The technique also gave good long- and short-term stabilities of under 6% RSD for both elements. A variety of samples, including water and urine standard reference materials, were analysed in both modes, and the precision and accuracy of the results for total arsenic and selenium levels were assessed. Using the technique in both modes also allowed for the fractionation of As and Se species into their volatile hydride-forming and non-hydride-forming species. This was particularly informative, with respect to As species present, in the case of a kelp powder extract. Digested tobacco samples were only analysed for their total As levels, in which case results obtained via both sample introduction modes showed good agreement.
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PMID:Sequential hydride generation/pneumatic nebulisation inductively coupled plasma mass spectrometry for the fractionation of arsenic and selenium species. 1896 6

A sequential arsenic extraction method was developed that yielded extraction efficiencies (EE) that were approximately double those using current methods for terrestrial plants. The method was applied to plants from two arsenic contaminated sites and showed potential for risk assessment studies. In the method, plants were extracted first by 1:1 water-methanol followed by 0.1M hydrochloric (HCl) acid. Total arsenic in plant and soil samples collected from contaminated sites was mineralized by acid digestion and detected by inductively coupled plasma-atomic emission spectrometry (ICP-AES) and hydride generation-atomic absorption spectrometry (HG-AAS). Arsenic speciation was done by high performance liquid chromatography coupled with HG-AAS (HPLC-HGAAS) and by HPLC coupled with ICP-mass spectrometry (HPLC-ICP-MS). Spike recovery experiments with arsenite (As(III)), arsenate (As(V)), methylarsonic acid (MA) and dimethylarsinic acid (DMA) showed stability of the species in the extraction processes. Speciation analysis by X-ray absorption near edge spectroscopy (XANES) demonstrated that no transformation of As(III) and As(V) occurred due to sample handling. Dilute HCl was efficient in extracting arsenic from plants; however, extraction and determination of organic species were difficult in this medium. Sequential extraction with 1:1 water-methanol followed by 0.1M-HCl was most useful in extracting and speciating both organic and inorganic arsenic from plants. Trace amounts of MA and DMA in plants could be detected by HPLC-HGAAS aided by the process of separation and preconcentration of the sequential extraction method. Both organic and inorganic arsenic compounds could be detected simultaneously in synthetic gastric fluid extracts (GFE) but EEs by this method were lower than those of the sequential method. The developed sequential method was shown to be reliable and applicable to various terrestrial plants for arsenic extraction and speciation.
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PMID:Extraction and speciation of arsenic in plants grown on arsenic contaminated soils. 1907 91

A method was developed for the simultaneous speciation of arsenic and antimony with HPLC-ICP-MS using C30 reversed phase column. Eight kinds of arsenic compounds (As(III), As(V), monomethylarsonic acid (MMAA), dimethylarsinic acid (DMAA), arsenobetaine (AB), arsenocholine (AsC), trimethylarsine oxide (TMAO) and tetramethylarsonium (TeMA)), Sb(III) and Sb(V) were simultaneously separated by the special mobile phase containing ammonium tartrate. Especially for the species of organic As, a C30 column was better than a C18 column in the effect of separation. Limits of detection (LOD) for these elements were 0.2 ng ml(-1) for the species of each As, and 0.5 ng ml(-1) for the species of each Sb, when a 10 microl of sample was injected, respectively. The proposed method was applied to a hot spring water and a fish sample.
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PMID:Study on simultaneous speciation of arsenic and antimony by HPLC-ICP-MS. 1907 53

Although metabolism of arsenicals to form methylated oxoarsenical species has been extensively studied, less is known about the formation of thiolated arsenical species that have recently been detected as urinary metabolites. Indeed, their presence suggests that the metabolism of ingested arsenic is more complex than previously thought. Recent reports have shown that thiolated arsenicals can be produced by the anaerobic microflora of the mouse cecum, suggesting that metabolism prior to systemic absorption may be a significant determinant of the pattern and extent of exposure to various arsenic-containing species. Here, we examined the metabolism of 34S labeled dimethylthioarsinic acid (34S-DMTA(V)) by the anaerobic microflora of the mouse cecum using HPLC-ICP-MS and HPLC-ESI-MS/MS to monitor for the presence of various oxo- and thioarsenicals. The use of isotopically enriched 34S-DMTA(V) made it possible to differentiate among potential metabolic pathways for production of the trimethylarsine sulfide (TMAS(V)). Upon in vitro incubation in an assay containing anaerobic microflora of mouse cecum, 34S-DMTA(V) underwent several transformations. Labile 34S was exchanged with more abundant 32S to produce 32S-DMTA(V), a thiol group was added to yield DMDTA(V), and a methyl group was added to yield 34S-TMAS(V). Because incubation of 34S-DMTA(V) resulted in the formation of 34S-TMAS(V), the pathway for its formation must preserve the arsenic-sulfur bond. The alternative metabolic pathway postulated for formation of TMAS(V) from dimethylarsinic acid (DMA(V)) would proceed via a dimethylarsinous acid (DMA(III)) intermediate and would necessitate the loss of 34S label. Structural confirmation of the metabolic product was achieved using HPLC-ESI-MS/MS. The data presented support the direct methylation of DMTA(V) to TMAS(V). Additionally, the detection of isotopically pure 34S-TMAS(V) raises questions about the sulfur exchange properties of TMAS(V) in the cecum material. Therefore, 34S-TMAS(V) was incubated and the exchange was monitored with respect to time. The data suggest that the As-S bond associated with TMAS(V) is less labile than the As-S bond associated with DMTA(V).
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PMID:Exploring the in vitro formation of trimethylarsine sulfide from dimethylthioarsinic acid in anaerobic microflora of mouse cecum using HPLC-ICP-MS and HPLC-ESI-MS. 1913 83


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