• Title/Summary/Keyword: gas mass spectrometer

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Evaluation of pesticide residue analysis of dieldrin in soil using a high resolution gas chromatograph/mass spectrometer (HR-GC/MS)

  • Hwang, Jae-Bok;Park, Tae-Seon
    • Korean Journal of Agricultural Science
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    • v.43 no.4
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    • pp.634-640
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    • 2016
  • The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

Simultaneous Analysis of Several Non-Steroidal Anti-Inflammatory Drugs in Urine by Gas Chromatograph/Negative Chemical Ionization-Mass Spectrometry (기체 크로마토그래프-질량분석법을 이용한 뇨중 비스테로이드성 소염진통제 (NSAIDs)의 동시 분석법)

  • Myung, Seung-Woon;Park, Joon-Ho;Kim, Myung-Soo;Cho, Hyun-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.571-576
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    • 1999
  • Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

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Volatile Components of Korean Native Tea Leaves (Camellia sinensis O. Kuntze) (한국(韓國) 자생차엽(自生茶葉)의 향기성분(香氣成分))

  • Park, Jang-Hyun
    • Korean Journal of Soil Science and Fertilizer
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    • v.30 no.3
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    • pp.295-300
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    • 1997
  • Flavor components of natively grown tea plant(Camellia sinensis O. kuntze) in Korea, collected from 12 locations, were analyzed by gas chromatograph and mass spectrometer. Seventy to eighty flavor components in tea leaves were separated by GC. Total 52 flavor components were identified by comparing gas chromatograhp retention time and mass spectral date. They were classified as 19 alcohols, 5 aldehydes, 2 hydrocarbons, 6 ketones, 4 esters, 3 lactones, 2 acids, 3 phenols, 4 pyrazines, and 4 nitrogenous compounds. Major compounds identified were geraniol, linalool oxide, 1-hexanol and ethanol.

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The study of chemical substances in Hymenoxys brachyactis(II) (Hymenoxys brachyactis의 화학성분에 관한 연구(II))

  • Lee, Sang-Jun;Kim, Sung-Han;Kim, Jung-Han
    • Applied Biological Chemistry
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    • v.38 no.5
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    • pp.473-477
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    • 1995
  • The dichloromethane extracts of the above ground parts of Hymenoxys brachyactis afforded three sesquiterpene lactones already reported, one new sesquiterpene lactone, biennin C and hispidulin as known toxic flavone. Structures of all compounds were established by spectroscopy and biennin C was determined as an adduct of the modified pseudoguanolide and hymenoxon by Gas Chromatograpy and MS spectrometer These sesquiterpene lactones have the same ${\alpha},{\beta}$-unsaturated functional group like that of hymenovin which has been known as major toxic constituent of important livestock poison. And biennin C is also considered as toxic compound because of toxic hymenoxon.

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Validation of an analytical method for cyanide determination in blood, urine, lung, and skin tissues of rats using gas chromatography mass spectrometry (GC-MS)

  • Shin, Min-Chul;Kwon, Young Sang;Kim, Jong-Hwan;Hwang, Kyunghwa;Seo, Jong-Su
    • Analytical Science and Technology
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    • v.32 no.3
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    • pp.88-95
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    • 2019
  • This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

Arson Fire Analysis Involving the Use of Flammable Liquilds as Accelerants (인화성액체를 촉진제로 사용한 방화화재의 감식기법에 관한 연구)

  • Choi, Min-Ki;Han, Dong-Hun;Choi, Don-Mook
    • Fire Science and Engineering
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    • v.28 no.4
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    • pp.64-72
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    • 2014
  • Flammable liquids residues in fire debris and pyrolysis products of flammable materials were analyzed by using Gas detecting tube, Gas Chromatograph/Mass Spectrometers (GC/MS), and Pyrolyzer. Comparison studies between chemical components detected in debris fired with and without Flammable liquids were performed. Though Flammable liquids were not present in debris, Gas detecting tube colors were also changed. Chemical components produced from conventional combustions were different from those produced from pyrolysis. Due to the difference of the reaction conditions between combustions and pyrolysis, different chemical products were produced. Petrochemical products of PVC wood-linoleum block could produce ignitable chemicals, such as toluene, ethylbenzene, undecane, and dodecane. So, for better fire investigation more consideration of those chemicals will be porformed.

Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry (EI-GC/MS/MS를 이용한 니트로사민류의 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.11
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    • pp.764-770
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    • 2014
  • This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

Etching Characteristics of ZnO Thin Films Using Inductively Coupled Plasma of HBr/Ar/CHF3 Gas Mixtures (HBr/Ar/CHF3 혼합가스를 이용한 ZnO 박막의 유도결합 플라즈마 식각)

  • Kim, Moon-Keun;Ham, Young-Hyun;Kwon, Kwang-Ho;Lee, Hyun-Woo
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.23 no.12
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    • pp.915-918
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    • 2010
  • In this work, the etching characteristics of ZnO thin films were investigated using an inductively coupled plasma(ICP) of HBr/Ar/$CHF_3$ gas mixtures. The plasma characteristics were analyzed by a quadrupole mass spectrometer (QMS) and double langmuir probe (DLP). The surface reaction of the ZnO thin films was investigated using X-ray photoelectron spectroscopy (XPS). The etch rate of ZnO was measured as a function of the $CHF_3$ mixing ratio in the range of 0-15% in an HBr:Ar=5:2 plasma at a fixed gas pressure (6mTorr), input power (700 W), bias power (200 W) and total gas flow rate(50sccm). The etch rate of the ZnO films decreased with increasing $CHF_3$ fraction due to the etch-blocking polymer layer formation.

Determination of selenium in milk powder by octopole reaction cell ICP-MS (Octopole Reaction Cell이 장착된 ICP-MS에 의한 분유 중 셀레늄의 정량)

  • Cho, Sung-Eel;Kim, Mi-Ju;Kim, Yong-Ha;Min, Young-Keun;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.203-210
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    • 2006
  • The determination of trace selenium in milk powder has been studied by octopole reaction cell(ORC)-ICP-MS. The interferences by polyatomic ions and other concomitant molecular species could be removed remarkably by using $H_2$ as reaction gas in ORC. Compared to the normal mode (no cell gas), the $H_2$ cell gas mode improved the accuracy and precision. The quantitative result was average 102.7% and it was slightly higher than certified standard value of milk powder and the RSD was 7.6%.

Determination of Mequitazine in Human Plasma by Gas-Chro-matography/Mass Spectrometry with Ion-Trap Detector and Its Pharmacokinetics after Oral Administration to Volunteers

  • Kwon Oh-Seung;Kim Hye-Jung;Pyo Heesoo;Chung Suk-Jae;Chung Youn Bok
    • Archives of Pharmacal Research
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    • v.28 no.10
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    • pp.1190-1195
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    • 2005
  • The objective of this study was to develop an assay for mequitazine (MQZ) for the study of the bioavailability of the drug in human subjects. Using one mL of human plasma, the pH of the sample was adjusted and MQZ in the aqueous phase extracted with hexane; the organic layer was then evaporated to dryness, reconstituted and an aliquot introduced to a gas chromatograph/mass spectrometer (GC/MS) system with ion-trap detector. Inter- and intra-day precision of the assay were less than 15.1 and $17.7{\%}$, respectively; Inter- and intra-day accuracy were less than 8.91 and $18.6{\%}$, respectively. The limit of quantification for the current assay was set at 1 ng/mL. To determine whether the current assay is applicable in a pharmacokinetic study for MQZ in human, oral formulation containing 10 mg MQZ was administered to healthy male subjects and blood samples collected. The current assay was able to quantify MQZ levels in most of the samples. The maximum concentration ($C_{max}$ was 8.5 ng/mL, which was obtained at 10.1 h, with mean half-life of approximately 45.5 h. Under the current sampling protocol, the ratio of $AUC_{t{\rightarrow}last}$ to $AUC_{t{\rightarrow}{\infty}}$ was $934{\%}$, indicating that the blood collection time of 216 h is reasonable for MQZ. Therefore, these observations indicate that an assay for MQZ in human plasma is developed by using GC/MS with ion-trap detector and validated for the study of pharmacokinetics of single oral dose of 10 mg MQZ, and that the current study design for the bioavailability study is adequate for the drug.