• Title/Summary/Keyword: GC-MS (SIM)

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Simultaneous Determination of Plasma Lactate, Pyruvate, and Ketone Bodies following tert-Butyldimethylsilyl Derivatization using GC-MS-SIM

  • Yoon, Hye-Ran
    • Biomedical Science Letters
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    • v.21 no.4
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    • pp.241-247
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    • 2015
  • Lactate and ketone bodies are considered biological markers for ketosis and several inherited metabolic disorders. In the current study, the specific ratios of lactate and ketone bodies as analytical tools for differential diagnosis of various lactic acidosis were devised. The study included a protein precipitation step following tert-butyldimethylsilyl derivatisation. Total run time was approximately 30 min including sample preparation and GS/MS analysis. The limits of detection were below 0.1 pg/mL over the targeted 4 analytes. The calibration curve was linear over the concentration range of $0.001{\sim}250{\mu}g/mL$ for pyruvate, beta-hydroxybutyrate, and acetoacetate ($R^2$ > 0.99). Inter-day accuracy and precision were 87.7~94.8% with RSD of 2.5~5.7% at 2 levels. Absolute recoveries (%) of target analytes were 87.0~98.4%. The method was validated for the quantification of lactate and ketone bodies for differentiation of lactic acidosis.

Characterization of Off-flavors from Film-Packed Soybean Sprouts (필름 포장된 콩나물의 유통 중 축적되는 이취의 종류 및 발생 특성)

  • Cho Kyoung-Shim;Kim Yong-Ho;Lee Young-Sang
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.51 no.3
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    • pp.220-226
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    • 2006
  • Soybean sprout is a traditional food and its market circulation as packed in a transparent film is increasing. To characterize the off-flavor produced from film-packed soybean sprouts, harvested soybean sprouts were stored at different temperature and oxygen conditions, and time-series changes in heads pace $O_2,\;CO_2$, ethanol (EtOH) concentrations as well as sensory off-flavor levels were measured. Lower temperature resulted in lower consumption of $O_2$, lower production of EtOH and less off-flavor. No off-flavors could be detected when atmospheric $O_2$ concentration was maintained over 4%, while alcoholic-flavor and off-flavor were initiated when $O_2$ decreased down to 2% and 1%, respectively. Under low $O_2$ conditions alcoholic-flavor following EtOH production preceeded prior to sensory off-flavor detection. Various aldehydes and fatty acids such as nonylaldehyde, decylaldehyde and stearic acid were identified by GC/MS from film-packed sprouts producing off-flavors. In conclusion to suppress off-flavor, soybean sprouts should be packed in a film which can control $O_2$ concentration over 2% and stored at low temperature around $4^{\circ}C$.

Flavor Composition of Garlic from Different Area (국내산 마늘의 향미성분)

  • Shin, Dong-Bin;Seog, Ho-Moon;Kim, Ji-Hyun;Lee, Young-Chun
    • Korean Journal of Food Science and Technology
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    • v.31 no.2
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    • pp.293-300
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    • 1999
  • Garlic from 4 main growing area was analyzed for the composition related to garlic flavor. Twenty-eight volatile compounds in garlic were separated by GC and twenty five were identified by GC/MS. Total peak area was high in garlic from $S\u{o}san$, and low from $Hampy\u{o}ng$. However, no significant difference was found in total peak area of sulfur compounds for garlic from Namhae, $S\u{o}san$, and $Uis\u{o}ng$. The results of free sugars analysis showed that relatively large amount of 1-kestose, 1-nystose, and 1-F-fructosyl nystose known as fructooligosaccharide were found in garlic in addition to glucose, fructose, and sucrose. Garlic from $S\u{o}san$ contained high amount of 1-nystose and 1-F- fructosyl nystose. Total free amino acid content in garlic was in a range of $2036.1{\sim}2704.0mg%$, and it was higher in garlic from $S\u{o}san$ and $Uis\u{o}ng$. Lactic acid, pyruvic acid, oxalic acid, malonic acid, fumaric acid, levunic acid, succinic acid, malic acid, citric acid and pyroglutamic acid were found in garlic. Total organic acid content in garlic was $1905.7{\sim}2359.2mg$, and garlic from $Hampy\u{o}ng$ had relatively low organic acid contents.

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Analysis of Characterization in Commercial Extra Virgin Olive Oils (유통 압착올리브유의 이화학적인 특성)

  • Nam, Ha-Young;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.7
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    • pp.866-873
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    • 2007
  • To analyze and differentiate volatile compounds of 13 extra virgin olive oils from market, solid-phase micro extraction (SPME) GC-MS and electronic nose (EN) equipped with metal oxide sensors were applied. The volatiles identified in extra virgin olive oils include hexanal, 4-hexen-1-ol, (Z)-3-hexen-1-ol, acetic acid, and 2,4-dimethyl-heptane, etc. Response from EN was analysed by the principal component analysis. Proportion of the first Principal component was 99.70%, suggesting that each aroma pattern of the 13 extra virgin olive oils could be discriminated by EN. Fatty acid compositions were oleic (61.1${\sim}$77.9 mole%), palmitic (11.7${\sim}$16.5 mole%), linoleic (4.7${\sim}$9.7 mole%), stearic (2.5${\sim}$2.9 mole%), Palmitoleic (0.8${\sim}$2.4 mole%), and linolenic acid (0.7${\sim}$1.2 mole%). In color study, extra virgin olive oil showed $L^{\ast}$ value of 81.7${\sim}$92.9, $a^{\ast}$ value of -28.3${\sim}$13.5 and $b^{\ast}$ value of 52.2${\sim}$139.0. Total phenol and ${\alpha}-tocopherol$ contents were 6.2${\sim}$24.9 mg/100 g and 5.5${\sim}$12.8 mg/100 g, respectively. In Rancimat test, the induction period of 13 extra virgin olive oils showed 31.76${\sim}$54.04 hr while their POV ranged from 13.5 to 22.9 meq/kg oil.

Toxicokinetics of 4-tert-octylphenol in rats (Rat에서의 Octylphenol의 독성동태 연구)

  • 손수정;강현구;이선우;서수경;박인숙;안미령;최홍석;조재민;손동환
    • Environmental Mutagens and Carcinogens
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    • v.21 no.2
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    • pp.122-127
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    • 2001
  • 4-tert-octylphenol (OP) is a surfactant additive widely used in the manufacture of a variety of detergents and plastic products. Also, OP is known to have estrogenic activity by interacting with development and functions of endocrine system. This study was carried out to obtain toxicokinetic parameters of OP in male Sprague-Dawley rats. Male rats were administered OP, by either single oral (gavage) applications of 50, 100 or 200 mg/kg body weight. or a single intravenous injections of 1, 5 or 10 mg/kg body weight. Blood samples taken at several time intervals after administration were obtained from the femoral artery. Analysis of blood samples for OP was performed by gas chromatography mass spectrometry (GC/MS). The detection limit of OP was 1.9 ng/$m\ell$ at SIM (selected ion monitoring) mode of GC/MS. Calibration curve for analysis of the concentrations of OP in plasma was (OP/butylphenol peak area ratio) = 0.0294 $\times$ (plasma cone.) + 0.028 ($r^2$= 0.9991). The OP plasma concentration was 3921 ng/$m\ell$ immediately after single intravenous application, decreased rapidly within 45 min, and was detectable at low concentration up to 6 hr after application. When administered orally in rats (50, 100 and 200 mg/kg), OP was detected in the blood early after gavage administration, indicating the rapid initial uptake from gastrointestinal tract, with Tmax obtained from 0.67~0.83 hr. Using the AUC (area under the curve) of plasma concentration vs. time, low oral bioavailabilities of 1.2, 5.0 and 5.3% were calculated for the 50, 100 and 200 mg/kg groups, respectively.

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Comparison Solid Phase Microextraction with Purge & Trap on the GC/MS Analysis of Volatile Organic Compounds in Biota Samples (Solid Phase Microextraction 및 Purge & Trap을 이용한 생물시료 중 휘발성 유기화합물의 GC/MS 분석비교)

  • Ahn, Yun-Gyong;Seo, Jong-Bok;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.392-399
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    • 2001
  • The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

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Polychlorinated Biphenyl Contaminations of Water, Soils and Sediments Sampled from Various Places of Korea (국내의 다양한 장소에서 채취된 수질, 토양 및 저질시료의 폴리염화비페닐에 의한 오염도)

  • Park, Hyun-Mee;Ryu, Jae-Chun;Kim, Young-Man;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.6
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    • pp.802-809
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    • 2000
  • Concentrations of polychlorinated biphenyl congeners (PCBs) in samples collected from 43 kindss of water, 35 kinds of soil and 11 kinds of sediment in various place of Korea have been monitored using GC/MS/SIM analytical method. In our investigation, mean recoveries were $83.8{\pm}10.4%$ for water, $94.9{\pm}12.2%$ for soil and sediment samples and $80.2{\pm}8.7%$ for the spiked $^{13}C{_{12}}$-PCBs. Detection limits of PCBs for water, soil and sediment samples are 0.01 ng/ml and 0.05 ng/g. PCB congeners in water samples were not detected within quantitation limit, but trace amounts were detected in most of soil and sediment samples. The contamination level of PCBs in Korea was evaluated to be lower than in advanced countries like USA, Europe and Japan.

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Development of Simultaneous Quantification Method of Phenylalkylamines in Oral Fluid (타액 중 페닐알킬아민유도체류의 일제분석법 확립)

  • Choi, Hye-Young;Baeck, Seung-Kyung;Jang, Moon-Hee;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.55 no.2
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    • pp.145-153
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    • 2011
  • A simultaneous detection and quantification method for determining the Phenylalkylamine derivatives, such as methamphetamine (MA), amphetamine (AM), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), ketamine (KT), norketamine (NKT), phentermine (PT), fenfluramine (FFA) and phenmetrazine (PM), in oral fluid was developed and validated according to international guidelines. The validated method was applied to actual oral fluid samples collected from drug abuse suspects. The recovery of phenylalkylamines from oral fluid collection devices was also assessed. Oral fluid specimens from 20 drug abuse suspects submitted by the police were collected using Salivette$^{TM}$, Quantisal$^{TM}$ or direct expectoration. The samples were screened using a biochip array analyzer. For confirmation, the samples were analyzed by GC-MS in selected-ion monitoring (SIM) mode after extraction using automated SPE with a mixed-mode cation exchange cartridge and derivatization with trifluoroacetic anhydride (TFAA). The results from the immunoassay were consistent with those from GC-MS. All the oral fluid samples gave positive results for MA, AM, PT and/or PM. The detection of phenylalkylamines in oral fluid can provide a better indication of recent use than urine or hair. Therefore, the oral fluid specimen was useful for demonstrating phenylalkylamines abuse in the driving under the influence of drug (DUID) as an alternative specimen for urine.

Characteristics of Bio-oil by Pyrolysis with Pig Feces (돈분을 이용한 열분해공정 바이오오일의 특성)

  • Kun, Zhu;Choi, Hong L.
    • Journal of the Korea Organic Resources Recycling Association
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    • v.16 no.4
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    • pp.57-63
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    • 2008
  • The characteristics of the bio-oil produced by the pyrolysis process with pig feces was investigated in this paper. The continuous auger-type reactor produced bio-oil was maintained at the temperature range of 400 to $600^{\circ}C$, which was higher than a typical that in a conventional pyrolysis system. The pig feces was used as the feedstock. The bio-oil and its compositions were characterized by water analysis, heating values, elemental analysis, bio-oil compounds, by Gas Chromatography/Mass Spectrometry (GC/MS), and functional group by $^1H$ NMR spectroscopy. It was found that the maximum bio-oil yields of 21% w.t. was achieved at $550^{\circ}C$. This result suggested that this auger reactor might be a potential technology for livestock waste treatment to produce bio-oil because it is able to be improved to reach higher efficiency of bio-oil production in further study. The pyrolysis system reported herein had low heat transfer into the feedstock in the auger reactor so that it needs improve the heat conduction rate of the system in further study.

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A Study on the determination of Residual Antibiotics and Synthetic Antibacterial Agents in Meas (II) - Simultaneous Gas Charomatography/Mass Spectrometry Analysis of Penicillin G, Chloramphenicol and Thiamphenicol - (식육중의 잔류 항생.항균제의 검정에 관한 연구 (II) - Penicillin G , Chloramphenicol, Thiamphenicol, Gas chromatography/Mass spectrometry 동시 분석 -)

  • 류재천;양종순;서지원;김명수;박종세
    • Journal of Food Hygiene and Safety
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    • v.8 no.1
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    • pp.9-15
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    • 1993
  • In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents in meat simultaneously, we studied a gas chromatography-mass spectrometry(GC/M8) analysis. For a simultaneous analysis of penicillin G, chloramphenicol and thiamphenicol in meat, a simple and rapid clean-up procedure including extraction with 0.01 M EDTA-2Na Mcilvaine buffer (pH 4.0), defatting with n-hexane, and elution with 0.01M-methanolic oxalic acid from Bond Elute $C_{18}$ cartridge, and quantitation by selected ion monitoring (SIM) mode after derivatization was performed. The recoveries (%) of penicillin G, chloramphenicol and thiamphenicol (CV, %) at 1 ppm fortification level were 63.5 (7.6), 76.3 (8.1) and 84.7 (2.0), and the detection limits of those were 0.6, 0.085 and $0.084\;\mu\textrm{g}$ beef, respectively. This method using 81M mode allows excellent detection and quantitation of residual antibiotics and antibacterial agents in meat. Moreover, confirmation by a full scan electron impact mass spectrum is possible if residual level in the sample in above 1 ppm.

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