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1.
Ellis JL Conklin SD Gallawa CM Kubachka KM Young AR Creed PA Caruso JA Creed JT 《Analytical and bioanalytical chemistry》2008,390(7):1731-1737
The simultaneous detection of arsenic and sulfur in thioarsenicals was achieved using xenon-based collision-cell inductively
coupled plasma (ICP) mass spectrometry (MS) in combination with high-performance liquid chromatography. In an attempt to minimize
the 16O16O+ interference at m/z 32, both sample introduction and collision-cell experimental parameters were optimized. Low flow rates (0.25 mL/min) and
a high methanol concentration (8%) in the mobile phase produced a fourfold decrease in the m/z 32 background. A plasma sampling depth change from 3 to 7 mm produced a twofold decrease in background at m/z 32, with a corresponding fourfold increase in the signal associated with a high ionization surrogate for sulfur. The quadrupole
bias and the octopole bias were used as a kinetic energy discriminator between background and analyte ions, but a variety
of tuning conditions produced similar (less than twofold change) detection limits for sulfur (32S). A 34-fold improvement in the 32S detection limit was achieved using xenon instead of helium as a collision gas. The optimized xenon-based collision cell
ICP mass spectrometer was then used with electrospray ionization MS to provide elemental and molecular-based information for
the analysis of a fortified sample of NIST freeze-dried urine. The 3σ detection limits, based on peak height for dimethylthioarsinic acid (DMTA) and trimethylarsine sulfide (TMAS), were 15 and
12 ng/g, respectively. Finally, the peak area reproducibilities (percentage relative standard deviation) of a 5-ppm fortified
sample of NIST freeze dried urine for DMTA and TMAS were 7.4 and 5.4%, respectively.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
2.
标准参考物质贻贝和虾样中砷和硒的氢化物发生-电感耦合等离子体发射光谱法测定 总被引:1,自引:0,他引:1
本文对标准参考物质贻贝和虾粉中砷和硒的测定作了较详细研究。用 HNO_3-HClO_4常压、HNO_3-HClO_4-HF 常压,HNO_3-HClO_4-HF 加压和王水-HClO_4加压消解四种样品处理方法的测定结果表明,前两种方法不能将有机物完全破坏,从而使砷和硒的测定结果偏低。用加压消解方法可使样品中的有机物基本破坏完全,砷和硒的测定结果与标准值基本吻合。本文还对高价氢化物元素的预还原等问题作了讨论。 相似文献
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Hydride generation atomic fluorescence spectrometry was for the first time utilized to determine trace toxic element arsenic in the skeleton fossils of four dinosaurs unearthed in Sichuan Province of China. The instrumental limit of detection (LOD) for arsenic was 0.03 μg/L under optimal experimental conditions, which compared favorably to that by ICP-AES and ETAAS. The samples were digested with aqua regia in boiling water bath. The recoveries of standard addition were found to be from 97 to 109%, and the analytical results were found in good agreement with those by ICP-AES. It is a simple, reliable, sensitive yet relatively inexpensive analytical method, compared to ICP-AES, ICP-MS or ETAAS. Interesting analytical results were found that the arsenic concentrations were all abnormally high in the skeleton fossils. The established analytical method and the analytical results may be helpful in revealing the mystery of the mass extinction of the dinosaur fauna. The analytical results, together with other data available to date, supported the argument that the arsenic toxicosis could be a contributing factor for the mass extinction of the dinosaur fauna in Sichuan Province of China. 相似文献
4.
Xi-Hong WuDai-Hai Sun Zhi-Xia ZhuangXiao-Ru Wang Hai-Fang GongJiang-Xing Hong Frank S.C Lee 《Analytica chimica acta》2002,453(2):311-323
The purpose of this study is to investigate the amounts and characteristics of heavy metals (As, Hg) leachable from several Chinese medicinal materials (CMM) under conditions simulating stomach and intestine digestion and absorption. Analysis by inductively coupled plasma mass spectrometry (ICP-MS) was compared with that by hydride generation atomic fluorescence spectrometry (HG-AFS). Focused microwave assisted extraction (MAE) and Soxhlet extraction were carried out to compare with the conventional sequential extraction method. The CMM studied included two mineral drugs: realgar and cinnabar, and two formulated drugs containing the two minerals. The leachable amounts of the target elements into artificial stomach fluid, artificial intestinal fluid, and artificial intestinal fluid in 0.5% trypsin were compared. The last solvent gave the greatest amounts of leachable As (0.41%) from realgar and Hg (1×10−4%) from cinnabar, but otherwise no significant effect on the leachable amounts was observed upon changing the following parameters: temperature (37-60 °C), HCl concentration (0.5-6 M), and CMM sample particle size (74 and 250 μm). The low leaching efficiencies observed confirmed the presence of As and Hg as insoluble species (sulfides)in these mineral drugs. Sequential extraction schemes were used to determine the species of mercury and arsenic in formulated drugs containing the minerals. Trace amounts of organic forms of arsenic (0.43%) and mercury (2.9×10−4%) were observed which could be the transformation products derived from the original cinnabar or realgar minerals in drug formulation. 相似文献
5.
A method for direct de termination of total in organic arsenic (III+V), arsenic (III) and dimethylarsinate (DMA) in sea water was developed by combining continuous‐flow selective hydride generation and inductively coupled plasma mass spectrometry (ICP‐MS) is presented. The principle underlying selective hydride generation is based on proper control of the reaction conditions for achieving separation of the respective arsenic species. The effects of pH and composition of reaction media on mutual interference between the arsenic species were investigated in detail. The results indicate that the appropriate media for the selective determination of total in organic arsenic, DMA and As(III) are 6 M HNO3, acetate buffer at pH = 4.63 and citrate buffer at pH = 6.54, respectively. The concentrations of total inorganic arsenic species, As(III+V), and As(III) were respectively deter mined and that of As(V) was obtained by the difference between them. As to the concentration of DMA, it was obtained after correction from the interference caused by As(III) and As(V). By following the established procedure, the detection lim its (as based on 3‐sigma criterion) for As(III+V), As(III) and DMA were 0.050, 0.009, and 0.002 ng/mL, respectively. There liability of the pro posed method was evaluated in terms of precision and spike addition. The results indicated that the precision of better than 3% and spike recovery of 95 to 105% for all the arsenic species tested in the natural sea water samples can be obtained. 相似文献
6.
Determination of trace lead by hydride generation-inductively coupled plasma-mass spectrometry 总被引:1,自引:0,他引:1
A newly developed hydride generation-inductively coupled plasma-mass spectrometry (HG-ICP-MS) system was employed to determine trace amounts of lead in geological and biological samples. Laboratory-made single-stage and double-stage gas-liquid separators (GLSs) were investigated in order to replace the consumable membrane-GLS. Possible reasons were given why double-stage GLSs were superior over the single-stage ones according to the factors such as GLS volume and configuration, carrier gas inlet mode and flow rate. Interferences in liquid and vapor phase from concomitant ions and their products were investigated employing different flow mani-folds. Memory effects contributed to the blank values, but could be reduced employing a special wash protocol. Internal and external standardization were combined to improve the accuracy of the method, with bismuth as the internal standard according to its similarity with lead in the HG-ICP-MS system. Compared with ICP-MS and hydride generation-atomic fluorescence spectrometry (HG-AFS) methods, the system performance of HG-ICP-MS was characterized with improved detection limit to 0.002 ng/ml and acceptable short- and long-term stabilities. The linear dynamic range of this method was up to 50 ng/ml lead. Three Chinese national certified reference materials: poplar leaves, human hair and copper ore, were analyzed for method validation, and the results agreed well with the certified values. At last, the method was also employed to determine wide range of lead concentrations in lightweight limestone and nervous tissue samples from infants of albino rats with recoveries between 95 and 105% (n=10). 相似文献
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Matoušek T Hernández-Zavala A Svoboda M Langrová L Adair BM Drobná Z Thomas DJ Stýblo M Dědina J 《Spectrochimica Acta Part B: Atomic Spectroscopy》2008,63(3):396-406
An automated system for hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer is described. Arsines are preconcentrated and separated in a Chromosorb filled U-tube. An automated cryotrapping unit, employing nitrogen gas formed upon heating in the detection phase for the displacement of the cooling liquid nitrogen, has been developed. The conditions for separation of arsines in a Chromosorb filled U-tube have been optimized. A complete separation of signals from arsine, methylarsine, dimethylarsine, and trimethylarsine has been achieved within a 60 s reading window. The limits of detection for methylated arsenicals tested were 4 ng l(-1). Selective hydride generation is applied for the oxidation state specific speciation analysis of inorganic and methylated arsenicals. The arsines are generated either exclusively from trivalent or from both tri- and pentavalent inorganic and methylated arsenicals depending on the presence of L-cysteine as a prereductant and/or reaction modifier. A TRIS buffer reaction medium is proposed to overcome narrow optimum concentration range observed for the L-cysteine modified reaction in HCl medium. The system provides uniform peak area sensitivity for all As species. Consequently, the calibration with a single form of As is possible. This method permits a high-throughput speciation analysis of metabolites of inorganic arsenic in relatively complex biological matrices such as cell culture systems without sample pretreatment, thus preserving the distribution of tri- and pentavalent species. 相似文献
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The use of hydride generation coupled with axial view inductively couple plasma atomic emission spectrometry was presented for the determination of selenium in plant samples. The chemical factors affecting potentially the hydride generation efficiency (hydrochloric acid, sodium borohydride and sodium hydroxide concentrations) were assessed through investigation of chemical interference, accuracy and repeatability. The accuracy of measurements was not affected by elements present in high concentration in the plant matrix (K, Ca, Mg, and P). No interference was also observed with transition metals. Using a real sample (maize) with standard additions, decreases of recoveries were sometimes observed for 0.1% (m/v) NaOH, and attained 13.8% in the most unfavourable case. The final accuracy of the method was verified by using two certified reference materials: CRM 402 (white clover) and CRM 279 (sea lettuce). No statistically significant differences were obtained between the measured concentrations and the certified values. The optimized method was found sensitive (detection limit 0.15 μg l−1), reliable and repeatable (R.S.D. between 1.3% and 4.0%). 相似文献
10.
Determination of tin in soil by continuous hydride generation and inductively coupled plasma mass spectrometry 总被引:2,自引:0,他引:2
A method was investigated for the determination of Sn in soil samples by KOH fusion followed by continuous hydride generation coupled with inductively coupled plasma mass spectrometry (HG-ICP-MS). Sample solutions in 3.0 M HCl were mixed in line with a solution of 2.4% NaBH4 and 0.25 M KOH to generate stannane gas. The mixture was delivered continuously to a gas/liquid separator and the stannane gas was introduced into a Perkin-Elmer Sciex Elan 6000 ICP-MS for concentration measurements. A method detection limit of 0.45 mg/kg was sufficient for Sn levels commonly found in soil samples. Sn concentrations as low as 2.5 mg/kg were reproducibly measured in soil samples. Sample results by HG-ICP-MS agreed within ±17% relative difference to results by instrumental neutron activation analysis (INAA) and within ±6% relative difference to results by KOH fusion followed by inductively coupled plasma optical emission spectroscopy (ICP-OES). 相似文献
11.
A simultaneous multi-elemental measurement of As, Bi, Ge, Sb, Se, and Sn was performed in this study by flow injection-hydride generation-inductively coupled plasma-time-of-flight mass spectrometry (FI-HG-ICP-TOFMS). An off-line pre-reduction treatment using a solution of 5% (m/v) KI and ascorbic acid for 15 min at 80 °C is described by presenting its advantages and disadvantages and compared with the results achieved without pre-reduction. Using optimised conditions the following figures of merit were achieved: limits of detection in the 0.08-0.54 ng ml−1 range and relative standard deviations (RSD) of 1.7-6.7%, respectively. Applying the presented method, two certified reference materials (NIST 1643d freshwater and PACS-2 marine sediment) were analysed to demonstrate the suitability of the method for analysis of real samples. Results obtained from treated samples showed good agreement with certified values while the untreated ones considerably departed from them. 相似文献
12.
This study aimed to establish complementary high performance liquid chromatography (HPLC) methods including three modes of separation: ion pairing, cation exchange, and anion exchange chromatography, with detection by inductively coupled plasma mass spectrometry (ICPMS). The ion pairing mode enabled the separation of inorganic arsenate (As(V)), monomethylarsonic acid (MMA(V)), and dimethylarsinic acid (DMA(V)). However, the ion pair mode was unable to differentiate inorganic arsenite (As(III)) from arsenobetaine (AsB); instead, cation exchange chromatography was used to isolate and quantify AsB. Anion exchange chromatography was able to speciate all of the aforementioned arsenic species. Potential inaccurate quantification problem with urine sample containing elevated concentration of AsB, which eluted immediately after As(III) in anion exchange or ion pairing mode, was overcame by introducing a post-column hydride generation (HG) derivatization step. Incorporating HG between HPLC and ICPMS improved sensitivity and specificity by differentiating AsB from hydride-forming arsenic species. This paper emphasizes the usefulness of complementary chromatographic separations in combination with HG-ICPMS to quantitatively determine concentrations of As(III), DMA(V), MMA(V), As(V), and AsB in the sub-microgram per liter range in human urine. 相似文献
13.
流动注射-氢化物发生-电感耦合等离子体原子发射光谱法测定矿石中的砷、锑、铋 总被引:2,自引:0,他引:2
本文将流动注射-氢化物-ICP/AES 技术应用于矿石中痕量砷、锑、铋的测定。结果表明,本法具有分析速度快(60样/小时),灵敏度高(As、Sb、Bi 的测定下限达μg/g 级),精度好及操作简便等优点。 相似文献
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选取了玉米秸秆与籽粒、小麦秸秆与籽粒、烟草等5种不同的植物样品,加入硝酸-过氧化氢,进行敞口消解,消解液中As(75As)采用电感耦合等离子体质谱仪He碰撞模式测定,以72Ge为内标元素。结果表明:2个国家生物成分分析标准物质GBW10011(GSB-2,小麦)和GBW10020(GSB-11,柑橘叶)砷的测定值在标准确认值范围内;在植物样品中加入砷标准溶液,加标回收率在87%~104%之间;方法检出限为0.0055 μg/g,灵敏度较高;对4个植物样品分别重复测定5次,相对标准偏差均小于10%。本文结论认为电感耦合等离子体质谱仪He碰撞模式可以用于测定硝酸-过氧化氢敞口消解植物样品中砷含量,该方法测定结果准确可靠,重现性好,灵敏度高。 相似文献
17.
A simple method for the speciation analysis of bio-accessible arsenic (As) in rice was developed using a continuous on-line leaching method to release the bio-accessible fraction. The continuous on-line leaching method has several advantages over commonly used batch methods including quicker and easier sample preparation, reduced risk of contamination and access to real time leaching data. The bio-accessibility of As in the samples was monitored using inductively coupled plasma mass spectrometry (ICP-MS). Results from a certified reference material as well as cooked and uncooked white rice showed that the majority of As was leached by saliva. Results obtained using the continuous on-line leaching method were comparable to those obtained using a batch method. Speciation analysis of the saliva leachate was performed using ion exchange chromatography coupled to ICP-MS. The four most toxic forms of As (As(III), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and As(V)) were clearly separated within 5 min in a single chromatographic run. Over 92% of bio-accessible As in the certified reference material and uncooked white rice sample was in the form of DMA and As(V), whereas it was present as DMA and As(III) in the cooked white rice. 相似文献
18.
Various toxicological and metabolic interactions have been reported to exist between arsenic and selenium. In the present
study, synthetic seleno-arsenic compounds, potentially suitable for probing metabolic interactions between these two elements,
were prepared and tentatively characterized by using high-performance liquid chromatography (HPLC)–electrospray tandem mass
spectrometry and HPLC–inductively coupled plasma mass spectrometry. In analogy to the recently identified thio-arsenic species,
which can be prepared from their corresponding oxo-arsenic species via reaction with H2S, the seleno-arsenic compounds were also derived from oxo-arsenic compounds via reaction with H2Se.
Figure H2Se bubbled into solutions containing oxo‐arsenosugars converts them into their seleno‐arsenosugar analogues. 相似文献
19.
等离子体光谱法同时测定羟基磷灰石中的As、Hg方法研究胡明芬童式国(四川大学分析测试中心成都610064)关键词砷汞等离子体光谱法氢化物发生羟基磷灰石[Ca5(PO4)3(OH),简称HA]是一种优良的生物活性材料,在医学上主要是制备各种人工骨制品,... 相似文献