• 제목/요약/키워드: Mass Spectrometric

검색결과 259건 처리시간 0.024초

GC/MSD를 사용한 원유 내 잔류농약의 분석법 연구 (Research for the Analytical Method of Various Pesticides in Raw Milk by Gas Chromatography-Mass Spectrometry)

  • 오남수;신용국;백승천
    • 한국축산식품학회지
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    • 제29권4호
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    • pp.482-486
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    • 2009
  • The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

Simultaneous Determination of Valproic Acid and its Toxic Metabolites, 4-ene-VPA and 2,4-diene-VPA in Rat Plasma using a Gas Chromatographic-mass Spectrometric Method

  • Lee, Min-Sun;Lee, Young-Joo;Chung, Bong-Chul;Jung, Byung-Hwa
    • Journal of Pharmaceutical Investigation
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    • 제40권3호
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    • pp.155-160
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    • 2010
  • A gas chromatographic-mass spectrometric (GC-MS) method was developed for the simultaneous determination of valproic acid (VPA) and its toxic metabolites, 4-ene-VPA and 2,4-diene-VPA in rat plasma. Extraction was performed in weak acidic condition (pH 5.2) to avoid degradation of 4-ene-VPA and 2,4-diene-VPA. The recoveries for 4-ene-VPA and 2,4-diene-VPA were more than 70% and that for VPA was 33-42%. R value for each compounds exceeded 0.998 in calibration curve during all the analysis. Accuracy and precision ranged from 88.3 to 113.2% and from 2.16 to 14.2%, respectively The method was successfully applied to monitor plasma concentrations of VPA, 4-ene-VPA and 2,4-diene-VPA after intravenous administration of VPA at the dose of 100 mg/kg, suggesting that these toxic metabolites may involved in the hepatotoxicity induced by VPA.

Correlations between Zirconium Isotopes and Burnup Parameters in PWR Spent Nuclear Fuels

  • Kim, Jung-Suk;Chun, Young-Shin;Lee, Chang heon;Kim, Won-Ho;Eom, Tae-Yun
    • 한국원자력학회:학술대회논문집
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    • 한국원자력학회 1998년도 춘계학술발표회논문집(2)
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    • pp.551-556
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    • 1998
  • The correlation of isotope composition of Zr with the turnup and some heavy isotopes in PWR uranium dioxide fuel has been investigated. The total and partial ($^{235}$ U) burnup were determined by $^{148Nd}$ and by U and Pu mass spectrometric method, respectively. After separating Zr from the fuel samples, its isotope composition was measured by mass spectrometry. In addition, the quantities of the U and Pu in the spent fuel were determined by isotope di lution mass spectrometric method using $^{233}$ U and $^{242}$ Pu as spikes. The content of some heavy isotopes, $^{235}$ U, $^{239}$ Pu and $^{241}$ Pu, and the Pu Contribution to total turnup were expressed by the correlation with Zr isotope ratios, $^{91}$ Zr/$^{96}$ Zr and $^{93}$ Zr/$^{96}$ Zr The correlations by isotope compositions measured were compared wi th those calculated from ORIGEN2 code.

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High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

  • Choi, Young-Wook;Nam, Dae-young;Kang, Kyoung-Hoon;Ha, Kyung-Wook;Han, In-Hee;Chang, Byung-Kon;Yoon, Mi-kyeong;Lee, Jae-hwi
    • Bulletin of the Korean Chemical Society
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    • 제27권2호
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    • pp.291-294
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    • 2006
  • A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC $C_{18}$ column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

Mass constraints of coronal mass ejection plasmas observed in EUV and X-ray passbands

  • 이진이
    • 천문학회보
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    • 제36권1호
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    • pp.39.1-39.1
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    • 2011
  • Coronal mass ejection (CME) plasmas have been observed in EUV and X-ray passbands as well as in white light. Mass of CME has been determined using polarized brightness observed by the Large Angle and Spectrometric Coronagraph Experiment (LASCO) on board Solar and Heliospheric Observatory (SOHO). Therefore, this mass obtained from the LASCO observation indicates the total CME mass. However, the mass of CME plasma in different temperatures can be determined in EUV and X-ray passbands using observations by SOHO/EIT, STEREO/EUVI, and Hinode/XRT. Prominence/CME plasmas have been observed as absorption or emission features in EUV and X-ray passbands. The absorption features provide a lower limit to cold mass. In addition, the emission features provide an upper limit to the mass of plasmas in temperature ranges of EUV and X-ray. We determine the mass constraints using the emission measure obtained by assuming the prominence/CME structures. This work will address the mass constraints of hot and cold plasmas in CMEs, comparing to total CME mass.

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Improved Calibration for the Analysis of Emerging Contaminants in Wastewater Using Ultra High Performance Liquid Chromatography and Time-of-Flight Mass Spectrometry

  • Pellinen, Jukka;Lepisto, Riikka-Juulia;Savolainen, Santeri
    • Mass Spectrometry Letters
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    • 제9권3호
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    • pp.77-80
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    • 2018
  • The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.