Parameters of InductivelyCoupledPlasmaMassSpectrometry (ICP-MS) (X-7, Thermo Electron Corporation of USA): Hoisting speed of sample 1.0 ml/min, atomizer cooling temperature 3˚C, Argon gas pressure 0.6 MPa. The other main parameters of ICP-MS have been presented in Table 1.
Laser ablation (LA) with inductivelycoupledplasmamassspectrometry (ICP-MS) is a powerful analytical technique that has been applied to multi- element analysis of trace, minor and major elements of solids in many areas of science including geological [1–3] , environmental [4-5] , medical [6-7] , biological [8-9] and forensic [10] as well as many other applications including semiconductor manufacturing [11-12] . In laser ablation, an intense laser pulse is used to remove a tiny mount of material from the irradiated sample [13–16] . Laser ablation is a complex process that is not fully understood. Many parameters involved in this process can interact in a complex way to make the processes of laser ablation complicated [17–24] . Wavelength, pulse width, fluence and repetition rate of the laser are among these parameters [25–30] . By decreasing the laser pulse width to the femtosecond (fs) range, mechanisms of laser-matter interaction become different. The non-linear mechanisms associated with fs laser ablation (avalanche and multiphoton ionization) are responsible for deterministic ablation behavior (i.e. well defined ablation threshold) and lower threshold fluence [31–33] . Ablation with fs laser pulses is less matrix-dependent and the produced particles have a narrower size distribution, with the maximum shifted toward the smaller size ranges compared to nanosecond (ns) laser ablation [34–36] .This improves the transport and ionization efficiencies of the ablated material during LA-ICP-MS analyses.
A droplet carrying particle is desolvation, vaporization, ionization, and dif- fusion in an inductivelycoupledplasma (ICP) to form a cloud of ions. It then is detected as a mass-spectrum peak of individual particle. The diameter of the particle is derived from its mass, which is calibrated using the peak area. This is the basic principle of measuring single particles using inductivelycoupledplasmamassspectrometry (ICP-MS). In this paper, a mathematical model describing single particles in plasma is investigated. This makes it possible to investigate the process and contributing factors of single particles measurement by ICP-MS. A series of processes are investigated, which in- clude increasing the droplet temperature to the boiling point, desolvation of the droplets, increasing the particle temperature to the melting point, the particles are melted from a solid to the liquid, increasing the particle tem- perature to the boiling point, and particle vaporization. The simulation shows that both the atomic (ion) diffusion in the plasma and the incomplete vaporization of the particles are two important factors that limit the signal intensity of the particle’s mass spectrum. The experiment reveals that ICP-MS is very linear for Ag nanoparticles below 100 nm and SiO 2 particles below
Major, minor, and trace elements in wines from the Republic of Macedonia were determined in this study. Both inductivelycoupledplasma–massspectrometry (ICP-MS) and inductivelycoupledplasma– optical emission spectrometry (ICP-OES) were used for accurate determination of the concentration of 42 elements (Ag, Al, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Ho, La, Lu, Mg, Mn, Mo, Na, Nd, Ni, P, Pb, Pr, S, Sm, Tb, Ti, Tl, Tm, U, V, Yb, Zn, Zr) in 25 Macedonian white, rose, and red wines from different wine regions. By means of factor and cluster analyses, the wines were discriminated according to wine type (white vs. red) and geographical origin. The main discriminant elements were B, Ba, Ca, Fe, Mg, Mn, P, and S.
Recently, we established novel laser ablation inductivelycoupledplasmamassspectrometry (LA-ICP-MS)-based protocols for hepatic metal bio-imaging. Here we demon- strate that these protocols are a significant asset in the diagnosis of iron overload allowing iron measurements with high sensitivity, spatial resolution, and quantification ability. These protocols will be valuable in estimating liver iron content in all forms iron imbalances resulting from genetic disorders (hemochromatosis, β -thalassemia, and aceruloplasminemia), iron malabsorption, internal chronic bleeding, excessive menstrual bleeding, and nutritional de- ficiencies resulting for example from strict vegetarian food consumption.
Abstract: The existence of elemental impurities in samples of pharmaceutical substances is a concern, not just due to significant toxic ity, and also due to the possible impact on drug stability, shelf - life, or undesired side effects. Elemental impurities therefore need to be carefully monitored and regulated. Metal contents in doxapram hydrochloride API were assayed by inductivelycoupledplasma - massspectrometry (ICP-MS). The doxapram hydrochloride active pharma ingredient (API) was analyzed for arsenic, cadmium, mercury, lead, vanadium, cobalt, nickel, copper, molybdenum, manganese, lithium, antimony, sodium and aluminum. The validation parameters like system suitability, specificity, linearity, LOD, LOQ, robustness, accuracy, precision, ruggedness and solution stability for the ICP-MS method was checked. Three batches of doxapram hydrochloride API was accessed by the validated ICP-MS method for the content of 14 selected elements. The method exhibited linearity in range of 0.425 - 3.40 ppb (cadmium), 1.25 - 10 ppb (lead and cobalt), 3.75 - 30 ppb (arsenic), 0.750 - 6.0 (mercury), 2.5 - 20 ppb (vanadium), 5.0 - 40.0 ppb (nickel), 22.5 - 180 ppb (antimony), 75 - 600 ppb (copper), 62.50 - 500 ppb (lithium), 375 - 3000 ppb (molybdenum) and 2500 - 20000 ppb (sodium, aluminium and manganese). The validation results are inside the limitations of criteria. All metals were found to be either below the detection limits or quantification limits except nickel in doxapram hydrochloride API. Analytical results of this investigation demonstrated that ICP-MS method validated is useful for monitoring the selected 14 metal impurities present in doxapram hydrochloride API.
The aim of this study is to estimate heavy metals in different brands of amlodipine besylate tablet dosage forms by inductivelycoupledplasma-massspectrometry (ICP-MS). In many laboratories around the world as the instrument of choice for performing trace metal analysis is ICP-MS. ICP-MS using Kinetic Energy Discrimination (KED) mode was used. Samples are assimilated using multi-wave sample digestion system. Each element standards of conc. 1000 mg/l was prepared and followed by serial dilution with 2% nitric acid. The validation was performed as per USP232 standards for the different brands of commercially available samples. Parameters such as linearity, accuracy, precision, Limit of detection (LOD), Limit of Quantification (LOQ) were evaluated. Calibration curves were linear and co-relation co-efficient (r 2 ) was 0.995 for all elements. LOD is divided into
Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethy- larsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductivelycoupledplasmamassspectrometry (LC-ICP-MS). Total arsenic concentrations in the samples ranged from 110 ng/gup to 420 ng/g. The i-As in the rice cereals accounted for 33% to 77% of the total arsenic. The observed variability between infant rice cereals makes a dietary survey approach to accessing arsenic exposures difficult.
In inductivelycoupledplasmamassspectrometry (ICP-MS) analysis, only a few options are available to deal with non-spectroscopic interferences. Considering that diluting the sample is impractical for traces analysis, other alternatives must be employed. Traditionally, the method of standard additions is used to correct the matrix effect but it is a time consuming method. Others methods involves separation techniques. Another way to overcome matrix interferences is to understand the mechanism involved and adjust plasma viewing conditions to reduce or eliminate the effect. In this study, the effect of various concomitant elements in ICP-MS was assessed by measuring the distribution of selected singly charged analyte ions (Al, V, Cr, Mn, Ni, Co, Cu, Zn, As, In, Ba, La, Ce, Pb), doubly charged ions (La, Ce, Ba and Pb) and oxides ions (BaO) in the presence of concomitant elements spanning a mass range from 23 (Na) to 133 (Cs) u.m.a. and different ionization energies. Concomitant elements are alkali metals, alkaline earth metals and Si. Analyte ion sup- pression was observed while moving the ICP across and away from the sampling interface with or without a single concomitant element. Matrix effect measures were realised, firstly, to highlight the relation between the signal extinction of an analyte and the masse of the concomitant element, and secondly to highlight the relation between the removal of the analyte signal and the first ionization energy of the element of matrix. A dependence upon both the mass of the matrix element and the mass of the analyte was observed. The sup- pression seems increased with increasing matrix element mass and decreased with increasing analyte mass. The effect of the mass of the matrix element was the more significant of the two factors. If space-charge ef- fects were found to be significant for matrix elements of much lower mass, it seems diffusion also played an active part for heavier matrix elements. Finally, some evidence was found for a shift in ion-atom equilibrium for dications and for energy demand regarding oxides.
We also measured Hf isotope ratios of in-house stand- ard solution JMC 14375, delivered from Alfa Aesar of Johnson Matthey Company (stock no. 14375, lot no. 83-084740F, plasma standard solution). The 176 Hf/ 177 Hf ratio of this standard solution (300 ng ml -1 Hf ), mea- sured with the same analytical design as that for the measurement of JMC 475 standard solution (20 cycles, 4.194 s integration) gave an average of 0.282228 ±0.000005 (n=10, 2σ S. E.) (Table 3).
Otoliths, which grow in daily increments in fish [9], can accurately record physical and chemical environmental conditions [10]. Otolith microchemistry is a method that has been recently applied to stock identification [11] [12] [13], and it can provide an understanding of the environmental history of fish move- ments [14], population structure [15], and the identification of spawning estu- aries [16]. Laser Ablation InductivelyCoupledPlasmaMassSpectrometry (LA-ICPMS) [17] [18] is a precision tool which could be used to analyze trace elements with solid materials. The high power pulsed laser beam is focused at selected locations on the otolith. In the laser ablation sampling system, the oto- lith grinding surface is ablated by a high-energy laser, and then the ions are ex- tracted with argon gas carried into the ICPMS for analysis [18] [19]. Previous studies have successfully discriminated among different stocks of Atlantic cod Gadus morhua using LA-ICPMS analysis of otolith nuclei, which demonstrated the variations in elemental concentrations [11]. The otolith forms in daily in- crements in larval-stage fish, with the first ring formed on the day of hatching [9]. Conversely, the external otolith reflects the wild environment after stocking. Microelements from the surrounding water bodies merge and precipitate onto the otolith, and other divalent ions ( i.e. Sr 2+ , Ba 2+ , Mg 2+ , etc.) may replace Ca 2+ in
The minimum inhibitory concentration of nanoparticles synthesized from aqueous seed extract of fenugreek was 5%. In the concluding remarks, the copper nanoparticles synthesized using fen[r]
ICP-MS instrument (iCAP Q, Thermo fisher scientific, USA) was used for measuring the concentration of elements in the digested sample solution under the following conditions: Plasma RF forward power 1548.6 W, sample uptake: 30 s, cool flow read back: 13.67 L/min, nebulizer flow: 1.0180 L/min, auxiliary flow read back: 0.796 L/min, integration time: 10 s, peristaltic pump speed: 40 rpm, sampler and skimmer cones: Ni, and analysis mode: eQuant.
The present work reports the simultaneous determination of macro-minerals and micro-minerals in the two selected seeds of wild date palm species (Phoenix sylvestris and Pheonix loureiroi) using inductivelycoupledplasmamassspectrometry (ICP-MS) and scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX).
Abstract: Naturally occurring radionuclides such as uranium, thorium and their decay products ( 226 Ra, 222 Rn) are present in a number of geological settings in Basrah Governorates. The uranium concentration of 78 soil samples using ICP-Mass (inductivelycoupledplasmamassspectrometry) was found to be ranging from 1.2 ppm in Eastern star1 to 15.75 ppm in AL-Liheise10 i n soils. The results are presented and compared with other studies . The measurements of uranium concentration of soils samples measured had a uranium content of less than 100 ppm, a concentration that characterizes overburden and tailings quality, rather than minable reserves. This paper presents and evaluates the concentration of uranium in Basrah Governorates .The study further reveals that 78 surface soil samples have uranium below detection limit.
Inductively coupled plasma mass spectrometry ICP-MS to quantitate the iron content after treatment for two hours with Hanks’ Balanced Salt Solution HBSS or 0.01 mM potassium ferricyanide[r]
the results suggest that the fibroblast DNA damage is not caused by the metal ions passing through the barrier. Instead the DNA damage may be a response to signalling molecules secreted by the trophoblast cells. This theory is supported by several pieces of evidence. (i) There was significantly increased DNA damage in fibroblasts exposed to the lowest concentration of metal ions indirectly across the barrier but DNA damage did not increase if the fibroblasts were exposed directly to the same concentration (Fig. 1c). (ii) Inductivelycoupledplasmamassspectrometry (ICP-MS) analysis showed no increase in total Co and Cr in the cell culture medium below barriers exposed to the lowest concentration of metal ions (Fig. 1d) but significantly increased DNA damage was detected in fibroblasts exposed to the lowest concentration of metal ions across the barrier. (iii) Exposure of the barriers to the middle and highest concentrations of metal ions led to a small increase of approximately 1 ppb of Cr in the media below the barrier (Fig. 1d). However there was no increase in DNA damage when fibroblasts were directly exposed either to 1 ppb Cr 6+ alone (Suppl. Fig. 2) or to 1.3 ppb Co 2+ and 2 ppb Cr 6+ (Fig. 1c). The trophoblast
technological advances. In this sense inductivelycoupledplasmamassspectrometry (ICP-MS) a multi-element technique with appropriate sensitivity is progressively replacing conventional techniques as atomic absorption or electrochemical methods (Fong et al., 2007; D’Ilio et al., 2008; Goullé et al., 2005; Zhou et al., 2002). Although these techniques may achieve the required sensitivity to determine elements at trace levels, they are lacking in speed and ease to use. ICP-MS could be very useful for a wide range of clinical applications because the great sensitivity acquired in this technique with low detection limits enabling toxicologists to sufficiently estimate the toxic levels and environmental metal exposure (Parsons and Barbosa Jr, 2007; Ammann, 2007; D’Ilio et al., 2006; Bárany et al., 1997; Rivero Martino et al., 2000; Sariego Muñiz et al., 1999). Furthermore, this method offers new possibilities in several fields such as clinical chemistry, clinical toxicology, forensic toxicology as well as workplace testing or environmental exposure and also applicable in epidemiological studies (Bortoli et al., 1992).The development of
is currently employed in the Olympic Dam processing plant (South Australia) to remove U and fluorine from copper concentrates prior to smelting but does not adequately remove the aforementioned RN. Due to chemical similarities between lead and alkaline earth metals (including Ra), two sets of experiments were designed to understand solution interactions between Sr, Ba, and Pb at various conditions. Nanoscale secondary ion massspectrometry (NanoSIMS) isotopic spatial distribution maps and laser ablation inductivelycoupled-plasmamassspectrometry transects were performed on laboratory-grown crystals of baryte, celestite, and anglesite which had been exposed to different solutions under different pH and reaction time conditions. Analysis of experimental products reveals three uptake mechanisms: overgrowth of nearly pure SrSO 4 and PbSO 4 on baryte; incorporation of minor of Pb and Ba into celestite due to diffusion; and extensive replacement of Pb by Sr (and less extensive replacement of Pb by Ba) in anglesite via coupled dissolution-reprecipitation reactions. The presence of H 2 SO 4 either enhanced or inhibited these reactions. Kinetic modelling supports the experimental results, showing potential for extrapolating the (Sr, Ba, Pb)SO 4 system to encompass RaSO 4 . Direct observation of grain-scale element distributions by nanoSIMS aids understanding of the controlling conditions and mechanisms of replacement that may be critical steps for Pb and Ra removal from concen- trates by allowing construction of a cationic replacement scenario targeting Pb or Ra, or ideally all insoluble sulfates. Experimental results provide a foundation for further investigation of RN uptake during minerals processing, especially during acid leaching. The new evidence enhances understanding of micro- to nanoscale chemical interactions and not only aids determination of where radionuclides reside during each processing stage but also guides development of flowsheets targeting their removal.