• 대한수의학회지
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• 제52권2호
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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.

• 한국대기환경학회지
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• 제21권4호
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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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• 제33권11호
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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.

• 생태와환경
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• 제52권4호
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• pp.324-332
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• 2019

본 연구는 Laser ablation ICP/MS (이하 LA-ICP/MS)를 이용한 환경오염 추적연구를 위하여 어류 내 이석을 분석하였다. 어류의 이석은 어류가 서식하는 환경에 영향을 받는 것으로 알려져 있어 국외에서는 이를 활용한 연구가 활발하나 국내에서는 이에 대한 연구가 미비한 실정이다. 그래서 본 연구에서는 환경오염의 지표로 사용되는 금속 원소의 성분 분석을 통하여 어류 이석을 이용한 환경오염 추적 가능성을 파악하고자 하였다. 또한 금속 원소의 성분 분석을 위해서는 전처리 과정을 줄여 분석 시간을 단축시킬 수 있는 것으로 알려진 LA-ICP/MS를 이용하였다. 시료채취는 연구지역과 배경지역으로 나누어 실험을 진행하였고, 실험 어종은 담수종인 잉어를 선정하였다. LA-ICP의 분석 최적 조건을 정립하기 위하여 이석 표준물질인 FEBS-1을 이용하여 9개 금속 원소(Li, Mg, Mn, Cu, Zn, Sr, Ba, Pb, U)의 정확도와 정밀도를 확인하였다. 정립한 조건을 이용하여 실제시료를 분석한 결과, 연구지역에서 채집한 어류 이석 내 금속 원소 성분의 총 농도가 2202.9 mg kg^-1으로 배경 지역의 1086.3 mg kg^-1보다 2.03배 높게 측정되었다. 원소별로는 Li과 U을 제외한 모든 원소가 연구 지역이 배경지역보다 높게 나타났다. 그리고 퇴적물 측정망 분석 자료와 비교한 결과, Zn, Pb, Cu가 두 지역의 퇴적물 금속 원소 농도 분포와 어류 이석 내 금속 원소 농도 분포 경향이 유사하게 나타났다. 이러한 결과로 보아 어류 내 이석은 퇴적물과 같이 환경오염원을 추적하는 데 활용할 수 있다는 것을 확인하였다.

• Mass Spectrometry Letters
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• 제6권4호
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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.

• 약학회지
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• 제36권3호
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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.

• 한국연초학회지
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• 제31권2호
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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 ${\pm}15%$.

• 분석과학
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• 제32권4호
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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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• 제26권3호
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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.

• 한국의류학회지
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• 제28권1호
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• pp.165-171
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• 2004

The analytical method of toxic heavy metals in disposable diapers was developed. Disposable diapers obtained from Korea, Japan, America and German were determinated and quantified. Sample treatment (Total Digestion) was wet chemical acid digestion for extraction of nine hazardous inorganic elements (Sb, As, Pb, Cd, Cr, Co, Cu, Ni, Hg) in disposable diapers. Inductively Coupled Plasma Mass Spectrometer (ICP-MS) and Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES) have been used for analyzing nine hazardous inorganic elements. The results were as follows : The concentration of extractable Sb which was treated for 3 hours with artificial urine and disposable diapers was higher than those of 6 hours and 24 hours. The concentration of extractable Cr was same as Sb. On the other hands, the behavior of Cu and Ni were different from Sb and Cr. Concentrations of extractable Cu and Ni increased as increasing the reaction time between artificial urine and disposable diapers.