摘要 :
Inarguably, one of the major issues concerning ICP-MS is spectral interferences. Around the year of 2000, some ICP-MS manufactures developed collision/reaction cells (CRCs) so as to cope with this issue. Since then, CRCs have unde...
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Inarguably, one of the major issues concerning ICP-MS is spectral interferences. Around the year of 2000, some ICP-MS manufactures developed collision/reaction cells (CRCs) so as to cope with this issue. Since then, CRCs have undergone continual refinments and improvement for nearly two decades, and eventually became vital devices in today's quadrupole ICP-MS. In this paper, the latest technological aspects of CRCs are reviewed and their fundamental limitations are clarified. Then follows a discussion about the mechanism for overcoming some of these limitaions by triple quadrupole ICP-MS (ICP-MS/MS). Particulary, this new technology enhances the capability of reaction cells by minimizing the cell-formed interferences and making the mass-shift method truly useful. Many of the interference problems that have remained unresolved for long in ICP-MS are now being resolved. The principles and applications of ICP-MS/MS are described in detail.
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The recent development and future prospects of trace elemental speciation by the on- line coupling of inductively coupled plasma mass spectrometry to separation methods, such as liquid chromatography, gas chromatography, supercrit...
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The recent development and future prospects of trace elemental speciation by the on- line coupling of inductively coupled plasma mass spectrometry to separation methods, such as liquid chromatography, gas chromatography, supercritical fluid chromatography, and capillary electrophosesis, are discussed. The extraction and derivatization methods of organometallic compounds in environmental and biological samples are also critically re- viewed.
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Mg/ Ca and Sr/Ca ratios in calcium carbonate are important components of many palaeoclimate studies. We present an isotope dilution method relying on a single mixed spike containing ~(25)Mg, ~(43)Ca and ~(87)Sr. Dozens of samples ...
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Mg/ Ca and Sr/Ca ratios in calcium carbonate are important components of many palaeoclimate studies. We present an isotope dilution method relying on a single mixed spike containing ~(25)Mg, ~(43)Ca and ~(87)Sr. Dozens of samples per day, as small as 10 lg of carbonate, could be dissolved, spiked and run in an ICP-MS with a precision of 0.8% (2 RSD). Two instruments types, a sector field and a quadrupole ICP-MS, were compared. The best long term precision found was 0.4% (2 RSD), although this increased by up to a factor of two when samples of very different Mg or Sr content were run together in the same sequence. Long term averages for the two instruments concurred. No matrix effects were detected for a range of Ca concentrations between 0.2 and 2 mmol l~(-1). Accuracy, tested by measuring synthetic standard solutions, was 0.8% with some systematic trends. We demonstrate the strength of this isotope dilution method for (a) obtaining accurate results for sample sets that present a broad Mg and Sr range and (b) testing solid carbonates as candidate reference materials for interlaboratory consistency. Mg/ Ca and Sr / Ca results for reference materials were in good agreement with values from the literature.
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Determination of trace element contents in crude oils constitutes a powerful geochemical tool, complementing organic geochemical analyses and allowing a deeper insight into the processes of oil generation, migration and maturation...
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Determination of trace element contents in crude oils constitutes a powerful geochemical tool, complementing organic geochemical analyses and allowing a deeper insight into the processes of oil generation, migration and maturation. Inductively coupled plasma mass spectrometry (ICP-MS) has been widely applied to trace element determination in petroleum samples due to its low detection limits and fast multi-element capability. However, quantification of several elements by quadrupole-based ICP-MS is hampered by low sensitivity due to high ionisation energy, severe polyatomic interferences and/or low abundance. In the present contribution an ICP tandem mass spectrometer (ICP-MS/MS), or triple quadrupole ICP-MS (ICP-QQQ-MS) has been used to overcome these limitations. Prior to analysis, samples were subjected to high pressure acid digestion, allowing external calibration by means of aqueous standards. 25 elements, including P, S, the first-row transition metals, As, Se, Re, Pb and U, could be quantified in one measurement. Polyatomic interferences on the lighter elements could be removed by reaction of the target ions with O-2 or NH3 in the collision/reaction cell of the ICP-MS/MS. The accuracy of the analytical method was assessed by the analysis of the standard reference materials NIST SRM 1634c (trace elements in fuel oil) and 1084a (wear-metals in lubricating oil). The measurement procedure was applied to the analysis of crude oil samples from the Alpine Foreland Basin of Austria. (C) 2016 Elsevier Ltd. All rights reserved.
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Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 Ps, re...
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Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 Ps, respectively, and wavelength of 785 nm were used to ablate NIST 610 synthetic glass and SRM 1107 Naval Brass B at the same spot for 800 to 1000 laser pulses at different repetition rates (5 to 50 Hz). Elemental fractionation was found to depend on repetition rate and showed a trend with femto econd laser ablation that is opposite to that observed in picosecond laser ablation for most measured isotopes. ICP-MS signal intensity was higher in femtosecond than picosecond LA-ICP-MS in both NIST 610 and naval brass when ablation was conducted under the same fluence and repetition rate. The differences irrsignal intensity were partly related to differences in particle size distribution between particles generated by femtosecortd and picosecond laser pulses and the consequent differences in transport and ionization efficiencies. The main reason for the higher signal intensity resulting from femtosecond laser pulses was related to the larger crater sizes compared to those created during picosecond laser ablation. Elemental ratios measured using Zn-66/Cu-63, (208)ph/U-238, Th-232/U-238, Zn-66/Th-232 and Zn-66/Pb-208 were found to change with the number of laser pulses with data points being more scattered in picosecond than femtosecond laser pulses. Reproducibility of replicate measurements of signal intensities, fractionation and elemental ratios was better for fs-LA-ICP-MS (RSD -3 to 6%) than ps-LA-ICP-MS (RSD -7 to 11%). (C) 2015 Elsevier B.V. All rights reserved.
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Due to the current demands in the fight against manipulation of blood and blood components, commonly referred to as "blood doping" in sports drug testing, specific and sensitive detection methods enabling the detection of prohibit...
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Due to the current demands in the fight against manipulation of blood and blood components, commonly referred to as "blood doping" in sports drug testing, specific and sensitive detection methods enabling the detection of prohibited substances and methods of doping are required. Similar to illicit blood transfusions, erythropoiesis stimulating agents have been shown to be misused in sport, aiming at improving an athlete's aerobic capacity and endurance performance. Amongst other strategies, the administration of ionic cobalt (Co2+) can increase the number of erythrocytes by stimulating the endogenous erythropoietin (EPO) biosynthesis. Conversely, several organic Co-containing compounds such as cyanocobalamin (vitamin B12) are not prohibited in sports, and thus, an analytical differentiation of permitted and banned contributions to urinary Co-concentrations is desirable. An excretion study with daily applications of either 1 mg of CoCl2 or 1 mg of cyanocobalamin was conducted with 20 volunteers over a period of 14 consecutive days. Urine, plasma, and concentrated red blood cells were analyzed for their cobalt content. The samples were collected starting 7 days before the administration until 7 days after. Total Co concentrations were analyzed by using inductively coupled plasma mass spectrometry (ICP-MS), which yielded significantly elevated levels exclusively after inorganic cobalt intake. Furthermore, a liquid chromatography (LC)-ICP-MS approach was established and employed for the simultaneous determination of organically bound and inorganic cobalt by chromatographic separation within one single run. The analytical approach offers the option to further develop detection methods of illegal Co2+ supplementation in sport.
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A multilaboratory validation (MLV) was performed to extend the U.S. Food and Drug Administration's (FDA) analytical method Elemental Analysis Manual (EAM) 4.10, High Performance Liquid Chromatography-Inductively coupled Plasma-Mas...
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A multilaboratory validation (MLV) was performed to extend the U.S. Food and Drug Administration's (FDA) analytical method Elemental Analysis Manual (EAM) 4.10, High Performance Liquid Chromatography-Inductively coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice, to include wine. Several method modifications were examined to optimize the method for the analysis of dimethylarsinic acid, monomethylarsonic acid, arsenate (AsV), and arsenite (AsIII) in various wine matrices with a range of ethanol concentrations by liquid chromatography-inductively coupled plasma mass spectrometry. The optimized method was used for the analysis of five wines of different classifications (red, white, sparkling, rose, and fortified) by three laboratories. Additionally, the samples were fortified in duplicate at levels of approximately 5, 10, and 30 kg(-1) and analyzed by each participating laboratory. The combined average fortification recoveries of dimethylarsinic acid, monomethylarsonic acid, and inorganic arsenic (iAs the sum of AsV and AsIII) in these samples were 101, 100, and 100%, respectively. To further demonstrate the method, 46 additional wine samples were analyzed. The total As levels of all the wines analyzed in this study were between 1.0 and 38.2 mu g kg(-1). The overall average mass balance based on the sum of the species recovered from the chromatographic separation compared to the total As measured was 89% with a range of 51-135%. In the Si analyzed samples, iAs accounted for an average of 91% of the sum of the species with a range of 37-100%.
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BackgroundComprehensive information on the effect of time and temperature storage on the measurement of elements in human, whole blood (WB) by inductively coupled plasma-dynamic reaction cell-mass spectrometry (ICP-DRC-MS) is lack...
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BackgroundComprehensive information on the effect of time and temperature storage on the measurement of elements in human, whole blood (WB) by inductively coupled plasma-dynamic reaction cell-mass spectrometry (ICP-DRC-MS) is lacking, particularly for Mn and Se. MethodsHuman WB was spiked at 3 concentration levels, dispensed, and then stored at 5 different temperatures: -70?°C, ?20?°C, 4?°C, 23?°C, and 37?°C. At 3 and 5?weeks, and at 2, 4, 6, 8, 10, 12, 36?months, samples were analyzed for Pb, Cd, Mn, Se and total Hg, using ICP-DRC-MS. We used a multiple linear regression model including time and temperature as covariates to fit the data with the measurement value as the outcome. We used an equivalence test using ratios to determine if results from the test storage conditions, warmer temperature and longer time, were comparable to the reference storage condition of 3?weeks storage time at ?70?°C. ResultsModel estimates for all elements in human WB samples stored in polypropylene cryovials at ?70?°C were equivalent to estimates from samples stored at 37?°C for up to 2?months, 23?°C up to 10?months, and ?20?°C and 4?°C for up to 36?months. Model estimates for samples stored for 3?weeks at ?70?°C were equivalent to estimates from samples stored for 2?months at ?20?°C, 4?°C, 23?°C and 37?°C; 10?months at ?20?°C, 4?°C, and 23?°C; and 36?months at ?20?°C and 4?°C. This equivalence was true for all elements and pools except for the low concentration blood pool for Cd. ConclusionsStorage temperatures of ?20?°C and 4?°C are equivalent to ?70?°C for stability of Cd, Mn, Pb, Se, and Hg in human whole blood for at least 36?months when blood is stored in sealed polypropylene vials. Increasing the sample storage temperature from ?70?°C to ?20?°C or 4?°C can lead to large energy savings. The best analytical results are obtained when storage time at higher temperature conditions (e.g. 23?°C and 37?°C) is minimized because recovery of Se and Hg is reduced. Blood samples stored in polypropylene cryovials also lose volume over time and develop clots at higher temperature conditions (e.g., 23?°C and 37?°C), making them unacceptable for elemental testing after 10?months and 2?months, respectively.
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ICP-MS and HPLC-ICP-MS were applied for diagnosis and therapeutic monitoring in a severe intoxication with a liquid containing hexavalent chromium (Cr(VI)) and inorganic arsenic (iAs). In this rare case a liver transplantation of ...
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ICP-MS and HPLC-ICP-MS were applied for diagnosis and therapeutic monitoring in a severe intoxication with a liquid containing hexavalent chromium (Cr(VI)) and inorganic arsenic (iAs). In this rare case a liver transplantation of was considered as the only chance of survival. We developed and applied methods for the determination of Cr(VI) in erythrocytes and total chromium (Cr) and arsenic (As) in blood, plasma, urine and liver tissue by ICP-MS. Exposure to iAs was diagnosed by determination of iAs species and their metabolites in urine by anion exchange HPLC-ICP-MS. Three days after ingestion of the liquid the total Cr concentrations were 2180 and 1070 mu g/L in whole blood and plasma, respectively, and 4540 mu g/L Cr(VI) in erythrocytes. The arsenic concentration in blood was 206 mu g/L. The urinary As species concentrations were <0.5, 109, 115, 154 and 126 mu g/L for arsenobetaine, As(III), As(V), methylarsonate (V) and dimethylarsinate (V), respectively. Total Cr and As concentrations in the explanted liver were 11.7 and 0.9 mg/kg, respectively. Further analytical results of this case study are tabulated and provide valuable data for physicians and toxicologists. (C) 2017 Published by Elsevier GmbH.
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Aim of this article is to review and discuss the currently used quantitative analytical method ICP-MS, which is used for quality control of pharmaceutical products. ICP-MS technique has several applications such as determination o...
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Aim of this article is to review and discuss the currently used quantitative analytical method ICP-MS, which is used for quality control of pharmaceutical products. ICP-MS technique has several applications such as determination of single elements, multi element analysis in synthetic drugs, heavy metals in environmental water, trace element content of selected fertilizers and dairy manures. ICP-MS is also used for determination of toxic and essential elements in different varieties of food samples and metal pollutant present in the environment. The Pharmaceuticals may generate impurities at various stages of development, transportation and storage which make them risky to be administered. Thus, it is essential that these impurities must be detected and quantified. ICP-MS plays an important function in the recognition and revealing of elemental impurities.
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