• Analytical Science and Technology
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• v.27 no.6
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• pp.269-276
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• 2014

A short study for the uncertainty of post column isotope dilution method has been performed for the analysis of Selenomethionine in HPLC-ICP/MS. Major error sources studied were concentration and the flow rate of Se isotope solution, atomic weights of Se in spike and sample, and isotope ratio measured for the spiked sample. Uncertainties were obtained for each factor and the contribution for the total concentration uncertainty was 54.4% and 0.61%, 0.0072% and 0.018%, and 45.0%, respectively. The biggest contribution factor was concentration of the spike solution and the second was the isotopic ratio measured for the spiked sample solution. The mass flow rate of spike and atomic weights did not show much contribution. The calculated total uncertainty was $1.46ng{\cdot}g^{-1}$ for the standard SeMet ($126.30ng{\cdot}g^{-1}$). The experimental result was $127.09{\pm}1.46ng{\cdot}g^{-1}$ and the relative uncertainty was 1.20%.

• Korean Journal of Veterinary Research
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• v.52 no.2
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• pp.69-74
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• 2012

The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

• Journal of Korean Society for Atmospheric Environment
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• v.21 no.4
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• pp.423-430
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• 2005

This study was investigated with sample digestion techniques and a reliability of the analytical results for a quantitative analysis of a standard reference material ('urban particulate matter', SRM 1648). The metallic elements were analyzed by inductively coupled plasma mass spectrometry (ICP-MS) with closed vessel microwave acid digestion method and atomic absorption spectroscopy (AAS). Quality control of the overall analytical procedures for metallic element determinations of standard reference material were estimated by analysis of a SRM 1648. Three digestion solutions $(type\;1:\;HNO_3,\;type\;2:\;HNO_3\;and\;H2O_2(4'1)\;mixture,\;type\;3:5.55\%\; HNO_3\;and\;16.75\%\;HCI\;mixture)$ were applied to SRM 1648. As a result, three digestion solutions used in this study are completely unable to digest Cr of SRM 1648. Reliability of Cr and As showed some errors in the digestion with digestion solution type (3) due to the influence of chlorides. Type (3) digestion solutions are sufficient to fulfill the digestion of As as well as Se in SRM 1648. ICP-MS results showed the improvement in accurate and precise determination of some trace elements like Cd, V and Pb in SRM 1648. It is important to use the proper digestion solution for each element to qualify analytical precision.

• Bulletin of the Korean Chemical Society
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• v.33 no.11
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• pp.3665-3670
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• 2012

Metal-p-$NH_2$-Bn-DOTA (paraammionobenzyl-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid: ABDOTA) complex was synthesized and purified for bio-tagging to quantify biological target materials using laser ablation (LA)-ICP-MS. Since the preparation of a pure and stable tagging complex is the key procedure for quantification, magnetic particles were used to purify the synthesized metal-ABDOTA complex. The magnetic particles immobilized with the complex attracted to a permanent magnet, resulting in fast separation from free un-reacted metal ions in solution. Gd ions formed the metal-complex with a higher yield of 64.3% (${\pm}3.9%$ relative standard deviation (RSD)) than Y ions, 52.3% (${\pm}2.5%$ RSD), in the pH range 4-7. The complex bound to the magnetic particles was released by treatment with a strong base, of which the recovery was 81.7%. As a reference, a solid phase extraction (SPE) column packed with Chelex-100 resin was employed for separation under similar conditions and produced comparable results. The tagging technique complemented polydimethylsiloxane (PDMS) microarray chip sampling in LA-ICP-MS, allowing determination of small sample volumes at high throughputs. For application, immunoglobulin G (IgG) was immobilized on the pillars of PDMS microarray chips and then tagged with the prepared Gd complex. IgG could then be determined through measurement of Gd by LA-ICP-MS. A detection limit of 1.61 ng/mL (${\pm}0.75%$ RSD) for Gd was obtained.

• Korean Journal of Ecology and Environment
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• v.52 no.4
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• pp.324-332
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• 2019

In this study, the possibility of a follow-up study on environmental pollution in domestic freshwater was identified by analyzing fish otoliths using Laser ablation-inductively coupled mass spectrometry (LA-ICP/MS). Fish otolith are known to be affected by the environment in which fish live. As a result, research on this subject is active in many countries; however, this is not the case in Korea. Therefore, in this study, the possibility of tracing environmental pollution using fish otoliths was identified by analyzing the components of metal elements used as indicators for environmental pollution. For the component analysis of metallic elements LA-ICP/MS, which can shorten analysis time by reducing the pretreatment process, was used. Sampling was conducted by dividing the research and the background area and carp, a freshwater species, was selected as the experimental fish species subject. Based on the established LA-ICP/MS conditions, the concentration of the metallic elements in the fish otoliths collected in the research area was 2202.9 mg kg^-1, 2.03 times higher than the 1,086.3 mg kg^-1 in the background area. All elements except for Li and U, were found to be higher in the research area than in the background area. Compared with the sediment measuring net analysis data, the distribution tendency of Zn, Pb, and Cu in sediment metal element concentrations in the two regions and distribution of metal element concentration in fish otoliths were similarly shown. These results confirm that fish otoliths can be used to track environmental pollutants, such as in sediments.

• Mass Spectrometry Letters
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• v.6 no.4
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• pp.85-90
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• 2015

This article reviews recent analytical techniques using inductively coupled plasma-mass spectrometry (ICP-MS) immunoassay for clinical and bio analysis. We classified the techniques into two categories, direct and indirect analysis, which depend upon a guideline of whether tagging materials are used or not. Direct analysis is well known, and generally used in conjunction with various other techniques, such as laser ablation, chromatographic separations, etc. Recently, indirect analysis using tagging elements has intensively been discussed because of its importance in future applications to bio and clinical analysis, including environmental and food industries. The method has shown advantages of multiplex detection, excellent sensitivity, and short analysis time owing to signal amplification and magnetic separation. Now, it expands the application field from small biomolecules to large cells.

• YAKHAK HOEJI
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• v.36 no.3
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• pp.199-204
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• 1992

The trace elements in animal feed were analyzed by Inductively Coupled Plasma Mass Spectrometer (ICP-MS, VG-PlasmaQuad Co.) to find possible sources of heavy metals accumulation in rat organ. The study about spectral interference was performed by analysis of a background spectrum of ICP-MS. Recovery test using standard of Cd and Se (100 ppb) was found to be better than 90%. Twenty elements (Ca, Fe, Mg, Ti, Cr, Ni, Cu, Zn, Ba, Al, Mn, Pb, B, Ce, Bi, U, V, Cd, and W)are determined.

• Journal of the Korean Society of Tobacco Science
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• v.31 no.2
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• pp.95-106
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• 2009

Semiquantitative analysis by ICP-MS has proven to be a powerful tool for fast screening, in addition, it does not require the element of interest to be present in the calibration standard, making it especially useful for the analysis of unknown samples. In this study, seven cigarette samples were analyzed by the rapid semi-quantitative analysis method based on the ICP-MS. For each cigarette sample, cut tobacco, cigarette paper, filter (before and after smoking), and smoke condensate were analyzed. The accuracy of the analysis technique was evaluated by comparing results obtained from Calibration Check Standard(CCS) and calibration method. Relative Percentage Error(RPE) value of all elements measured for three CCS showed a stable result of less than ${\pm}20%$. Compared to full quantitative analysis by calibration method, the results for cigarette samples showed average error within ${\pm}15%$.

• Analytical Science and Technology
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• v.32 no.4
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• pp.121-130
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• 2019

Alumina is one of the most important ceramic materials because of its useful physical and chemical properties. Recently, high-purity alumina has been used in various industrial fields. This leads to increasing demand for reliable elemental analysis of impurities in alumina samples. However, the chemical inertness of alumina makes the sample preparation for conventional elemental analysis a tremendously difficult task. Herein, we demonstrated the feasibility of laser ablation for effective sampling of alumina powder. Laser ablation performs sampling rapidly without any chemical reagents and also allows simultaneous optical emission spectroscopy and mass spectrometry analyses. For six alumina samples including certified reference materials and commercial products, laser-induced breakdown spectroscopy (LIBS) and laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) analyses were performed simultaneously based on a common laser ablation sampling. LIBS was found to be useful to quantify alkali and alkaline earth metals with limits-of-detection (LODs) around 1 ppm. LA-ICP-MS could quantify transition metals such as Ti, Cu, Zn, and Zr with LODs in the range from a few tens to hundreds ppb.

• Bulletin of the Korean Chemical Society
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• v.26 no.3
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• pp.440-446
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• 2005

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.