• Title/Summary/Keyword: GC/MS spectrometry

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Transformation of dissolved organic matter in a constructed wetland: A molecular-level composition analysis using pyrolysis-gas chromatography mass spectrometry

  • Park, Jongkwan;Choi, Mijin;Cho, Jaeweon;Chon, Kyongmi
    • Environmental Engineering Research
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    • v.23 no.4
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    • pp.390-396
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    • 2018
  • This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

Volatile Compounds for Discrimination between Beef, Pork, and Their Admixture Using Solid-Phase-Microextraction-Gas Chromatography-Mass Spectrometry (SPME-GC-MS) and Chemometrics Analysis

  • Zubayed Ahamed;Jin-Kyu Seo;Jeong-Uk Eom;Han-Sul Yang
    • Food Science of Animal Resources
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    • v.44 no.4
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    • pp.934-950
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    • 2024
  • This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

Constructing Database for Drugs and its Application to Biological Sample by HPTLC and GC/MS (HPTLC와 GC/MS를 이용한 의약품의 데이타베이스화 및 생체시료에의 응용)

  • Yoo, Young-Chan;Park, Sung-Woo;Lim, Mie-Ae;Baeck, Seung-Kyung;Park, Seh-Youn;Lee, Ju-Seon;Lho, Dong-Seok
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.136-150
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    • 2000
  • For the identification of unknown drugs in biological samples, we attempted rapid high performance thin layer chromatographic method which is sensitive and selective chromatographic analysis of high performance thin layer chromatography (HPTLC) with automated TLC sampler and ultra-violet (UV) scanner. We constructed HPTLC database (DB) on two hundred five drugs by using the data of Rf values and UV spectra (scan 200-360 nm) as well as gas chromatography/mass spectrometry (GC/MS) DB on ninety six drugs by using the data of relative retention time (RRT) on lidocain and mass spectra. After extracting drugs in biological sample by solid phase extraction (Clean Screen ZSDAU020), we applied them to HPTLC and GC/MS DB. Drugs, especially extracted from biological samples, showed good matching ratio to HPTLC DB and these drugs were confirmed by GC/MS. In conclusion, this DB system is thought to be very useful method for the screening of unknown drugs in biological samples.

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Structural Analyses of the Novel Phosphoglycolopids Containing the Unusual very Long Bifunctional Acyl Chain, α,ω-13,16-Dimethyloctacosanedioate in Thermoanaerobacter ethanolicus

  • Lee, Sang-Hoo;Kang, Se-Byung;Kim, Jai-Neung;Jung, Seun-Ho
    • Bulletin of the Korean Chemical Society
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    • v.23 no.12
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    • pp.1778-1784
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    • 2002
  • Novel membrane lipids containing the unusual very long chain fatty $acid{\alpha}{\omega}-1316-dimethyloctacosanedioate$, dimethyl. Ester (DME C30) was isolated and purified from thermophilic anaerobic eubacterium, Thermoanaerobacter ethanolicus. Structures of the lipids containing the bifunctional fatty acyl components were proposed by various analyses such as $^1H,\;^{13}C,\;^{31}P$ nuclear magnetic resonance (NMR), Fourier transform infrared(FTIR) spectroscopy, gas chromatography/mass spectrometry (GC/MS) and fast atom bombardment mass spectrometry (FAB/MS). Combined with the GC/MS, $^1H,\;and\;^{13}C$NMR data, we confirmed that the head groups of the lipids contained the glycerol and/or glucosamine molecules. $^{31}P$ NMR spectrum also showed that the lipids contained phosphate in a phosphodiester linkage. The proposed structures of these novel lipid components were the ones in which two head groups were linked by the membrane spanning fatty acyl component(DME C30)and regular chain fatty acids on glycerol moiety of each head group.

Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS (HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법)

  • Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun;Yeom, Hye-Sun;Lee, Sang-Ki;Park, Yoo-Sin;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.429-440
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    • 2010
  • HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Simultaneous determination of amphetamine derivatives and norketamine in hair by GC-MS/MS (GC-MS/MS를 이용한 모발 중 암페타민 유도체 및 노르케타민 동시분석)

  • Kim, Jin Young;Shin, Soon Ho;Ko, Beom Jun;Chung, Jae Cheol;Suh, Yong Jun;In, Moon Kyo
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.210-218
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    • 2009
  • A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and validated for simultaneous determination of amphetamine derivatives and norketamine in human hair. Preparation of hair involves external decontamination, mechanical pulverization, incubation and extraction prior to instrumental analysis. The samples were derivatized using heptafluorobutyric anhydride, and analyzed by GC-MS/MS. The linear ranges were 0.05-20.0 ng/mg for the analytes except for 3,4-methylenedioxyamphetamine, with good coefficients of determination ($r^2$ >0.998). The intra-day and inter-day precisions were within 10.7% and 8.5%, respectively. The intra-day and inter-day accuracies were between -1.6 and 17.0% and -2.6 and 10.5%, respectively. The limits of detections for each analyte were lower than 0.007 ng/mg, while recoveries were 75.9-100.9%. When the method was applied to hair samples obtained from suspected drug abusers, the concentrations in hair samples were 0.97-19.30 ng/mg for methamphetamine and 0.14-2.56 ng/mg for amphetamine.

Insecticidal Activity of Spearmint Oil against Trialeurodes vaporariorum and Bemisia tabaci Adults (온실가루이와 담배가루이에 대한 Spearmint Oil의 살충활성)

  • Choi Yu-Mi;Kim Gil-Hah
    • Korean journal of applied entomology
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    • v.43 no.4 s.137
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    • pp.323-328
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    • 2004
  • These studies were carried out to investigate the fumigation and contact toxicities of spearmint oil (Mentha spicata) against adults of greenhouse whitefly, Trialeurodes vaporariorum and sweet-potato whitefly, Bemisia tabaci. And we carried out the constituent analysis of spearmint oil using gas chromatograph (GC) and gas chromatograph mass spectrometry (GC/MS). Spearmint oil showed $99.1\%,\;91.7\%,\;41.1\%$ fumigation toxicity against T. vaporariorum adults at $10{\mu}L/954mL,\;5{\mu}L/954mL,\;1{\mu}L/954mL$ air concentration, respectively. In case of B. tabaci adults, spearmint oil showed $100\%,\;100\%,\;61.3\%$ fumigation toxicity, respectively. However, spearmint oil showed < $30\%$ contact toxicity against adults of T. vaporariorum and B. tabaci. Through the constituent analysis using GC and GC/MS, we confirmed main constituents of spearmint oil were limonene ($16.1\%$), ${\gamma}$-terpinene($13.8\%$), ${\rho}$-cymene($5.8\%$), 3-octanol($6.9\%$), carvone($40.9\%$). Carvone, major constituent of spearmint oil, also showed $100\%$ fumigation toxicity at $10{\mu}L/954mL$ air concentration.

Partial Reduction of Dinitroaniline Herbicide Pendimethalin by Bacillus sp. MS202 (Bacillus sp. MS202에 의한 Dinitroaniline계 제초제인 Pendimethalin의 부분환원)

  • Lee, Young-Keun;Chang, Hwa-Hyoung;Jang, Yu-Sin;Hyung, Seok-Won;Chung, Hye-Young
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.197-202
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    • 2004
  • The persistence of pendimethalin in soil and ground water has an injurious effect on ecosystem. Pendimethalin-degrading bacterium was isolated from Masan, Gyeongnam province and temporarily identified as Bacillus sp. MS202 by the analysis of API CHB50, kit, FAME, and 16S rDNA sequence. from the analysis of pnedimethalin metabolite using TLC, GC, and GC-MS, we found that the degradation of pendimethalin by Bacillus sp. MS202 did not result in the dealkylated form, but the formation of the reduced compound, 6-amino-2-nitro-N(1-ethylpropyl)-3,4-xylidine or 2- amino-6-nitro-N(1-ethylpropyl)-3,4-xylidine.

Removal of residual VOCs in a collection chamber using decompression for analysis of large volatile sample

  • Lee, In-Ho;Byun, Chang Kyu;Eum, Chul Hun;Kim, Taewook;Lee, Sam-Keun
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.23-35
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    • 2021
  • In order to measure the volatile organic compounds (VOCs) of a sample which is too large to use commercially available chamber, a stainless steel vacuum chamber (VC) (with an internal diameter of 205 mm and a height of 50 mm) was manufactured and the temperature of the chamber was controlled using an oven. After concentrating the volatiles of the sample in the chamber by helium gas, it was made possible to remove residual volatile substances present in the chamber under reduced pressure ((2 ± 1) × 10-2 mmHg). The chamber was connected to a purge & trap (P&T) using a 6 port valve to concentrate the VOCs, which were analyzed by gas chromatography-mass spectrometry (GC-MS) after thermal desorption (VC-P&T-GC-MS). Using toluene, the toluene recovery rate of this device was 85 ± 2 %, reproducibility was 5 ± 2 %, and the detection limit was 0.01 ng L-1. The method of removing VOCs remaining in the chamber with helium and the method of removing those with reduced pressure was compared using Korean drinking water regulation (KDWR) VOC Mix A (5 μL of 100 ㎍ mL-1) and butylated hydroxytoluene (BHT, 2 μL of 500 ㎍ mL-1). In case of using helium, which requires a large amount of gas and time, reduced pressure ((2 ± 1) × 10-2 mmHg) only during the GC-MS running time, could remove VOCs and BHT to less than 0.1 % of the original injection concentration. As a result of analyzing volatile substances using VC-P&T-GC-MS of six types of cell phone case, BHT was detected in four types and quantitatively analyzed. Maintaining the chamber at reduced pressure during the GC-MS analysis time eliminated memory effect and did not affect the next sample analysis. The volatile substances in a cell phone case were also analyzed by dynamic headspace (HT3) and GC-MS, and the results of the analysis were compared with those of VC-P&T-GC-MS. Considering the chamber volume and sample weight, the VC-P&T configuration was able to collect volatile substances more efficiently than the HT3. The VC-P&T-GC-MS system is believed to be useful for VOCs measurement of inhomogeneous large sample or devices used inside clean rooms.

Changes volatile flavor components of Korean Agrimonia Japonica by cooking (조리에 따른 한국산 짚신나물(Agrimonia Japonica)의 휘발성 풍미 성분의 변화)

  • 이혜정;이경희;구성자
    • Korean journal of food and cookery science
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    • v.11 no.2
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    • pp.122-125
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    • 1995
  • An attempt was made to determine the effect of the volatile components of edible wild grass by cooking. We collect the volatile components of Agrimonia Japonica by dynamic\ulcorner head space method. Samples were analyzed by gas chromatography-mass spectrometry(GC-MS). Thirty-six components, including 16 hydrocarbons, 7 alcohols, 4 esters, 7 benzoid compounds, 1 aldehyde and 1 ketone were confirmed in raw samples. Also 6 hydrocarbons identified in cooked sample. Alpha-pinene and 3-he-xane-ol were regarded as the most abundant components in raw sample. By heating of Japonica, most of the volatile compounds were disappeared, but alpha-pinene was remained abundantly.

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