• Title/Summary/Keyword: GC-O

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Determination of the PDE-5 Inhibitors and Their Analogues by GC-MS and TMS Derivatization

  • Pyo, Jae-Sung;Lee, Hee-Sang;Park, Yu-Jin;Jo, Ji-Yeong;Park, Yong-Hoon;Choe, Sang-Gil;Lee, Mi-Young;Lee, Jae-Sin
    • Mass Spectrometry Letters
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    • v.3 no.1
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    • pp.15-17
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    • 2012
  • Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

Analysis of Higenamine Contents in Plants with HPLC and GC/MSD (HPLC 및 GC/MSD를 이용한 식물 중의 Higenamine 함량 분석)

  • YunChoi, Hye-Sook;Suh, Young-Bae;Hahn, Young-Hee;Song, Yun-Seon;Ryu, Jae-Chun;Chung, Kyo-Soon
    • Korean Journal of Pharmacognosy
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    • v.29 no.2
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    • pp.129-135
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    • 1998
  • Higenamine is known as a cardiotonic principle of Aconiti tuber. The analytical procedures were established for the detection of higenamine in plants. The amounts of higenamine in several Aconiti tubers and the embryo of Nelumbo nucifera, another plant species known to contain higenamine, were determined. The $H_2O$ soluble fraction prepared from MeOH extract was first treated with AD-2 resin and then applied to either HPLC or GC/MSD systems. With HPLC, $6.4{\sim}19.2\;{\mu}g/g$ of higenamine were detected from various Aconiti tubers and $182.3\;{\mu}g/g$ of higenamine from the embryo of Nelumbo nucifera. The results obtained with GC/MSD also provided comparable data with those obtained with HPLC.

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Screening procedure for organochlorinated pesticide residues in meat fat using a matrix solid phase dispersion(MSPD) extraction and GC/ECD (MSPD법과 GC/ECD를 이용한 식육중의 잔류농약 분석)

  • 백미순;이영철;박병옥;김창수;박유순
    • Korean Journal of Veterinary Service
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    • v.22 no.1
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    • pp.15-23
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    • 1999
  • A multiresidue, simple and rapid isolation technique known as matrix-solid phase dispersoin (MSPD) for the extraction and quantitative gas chromatographic/electron capture detection (GC/ECD) determination of 14 organochlorinated pesticides($\alpha$-BHC, ($\beta$-BHC, ($\gamma$-BHC, aldrin, dieldrin, endrin, heptachlor, ($\alpha$-endosulfan, ($\beta$-endosulfan, endosulfan sulfate, p,p'-DDE, o,p'-DDD, p,p'-DDD, p,p'-DDT) from meat fats. The 14 pesticide were fortified into meat fat(0.5g) and blend with 2g $C_{18}$, $C_{18}$meat fat matrix blend and 2g activated florisil comprise an extraction column from which the pesticides are eluted by adding 8ml acetonitrile. Then 2${\mu}\ell$ of the eluate is analyzed by GC/ECD. Unfortified blank controls are tested similarly. The eluate contained all the pesticide analytes and was free of interfering coextractants. Recovery rate(31.3-500ng/g) were ranged from 80$\pm$4% to 97$\pm$4%. Any organochlorinated pesticides were not detected in 120 samples of beef and pork collected from slaughter houses in Kyeonggi province.

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Determination of urinary metabolite of IBP after oral administration and dermal application to rats (흰쥐를 이용한 IBP의 경구투여 및 피부도포 후 요중 대사물질 측정)

  • Min Kyung Jin;Cho Young Joo;Cha Chun Geun
    • Journal of Environmental Health Sciences
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    • v.28 no.1
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    • pp.67-77
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    • 2002
  • This study was aimed to determine the urinary metabolite of IBP, one of the organophosphorus pesticides, as the biomarkers of exposure. Urine samples were collected for 24 hours in metabolic cages after oral administration and dermal application of IBP to rats. Identification of the derivatized urinary metabolite was determined by GC/MS and excretion time courses of the urinary metabolite was analyzed by GC/FPD. Urinary metabolite o IBP, diisopropyl phosphorothioate, was detected in rats urine both after oral administration and dermal application of IBP. Parent compound was not detected in the experiment. In GC/MS, the mass spectral confirmation for diisopropyl phosphorothioate ion was identified at m/z 254. Diisopropyl phosphorothioate was excreted within 48 hours and 72 hours after oral administration and dermal application of IBP, respectively. In this study, the same urinary metabolite of IBP was detected both in oral and dermal exposure. Generally, excretion of the urinary metabolite after oral administration was faster than after dermal application. It is suggested that urinary diisopropyl phosphorothioate could be used as the biomarkers of exposure to IBP.

Determination of the mole fractions of ethylene oxide and freons in medical liquefied gas mixture by GC/AED (GC/AED를 이용한 의료용 액화혼합가스 중 산화에틸렌 및 프레온 가스류의 몰분율 측정)

  • Kim, Hyunjoo;Kim, Dalho;Lim, Arang;Lee, Taeck-Hong;Kim, Jin Seog
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.382-387
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    • 2012
  • Ethylene oxide ($C_2H_4O$, EtO) is used as a raw material for the production of ethylene glycol and other industrially important material such as ethanolamines and also used as a disinfecting agent. It is applied for gas-phase sterilization of thermally sensitive medical equipment, and for processing of storage facilities as a mixture with fluorinated hydrocarbon. In this perspective, accurate determination of the mole fractions of components in the liquefied gas mixture is required for the quality control and safety of production and use. Each component of the liquefied gas mixture has different chemical and physical properties such as vapor pressure and boiling point. Therefore, we can suppose that analytical results can be different according to the introduction method for the gas phase of upper layer, or for the liquid phase of lower layer in gas cylinder. In this study, we designed a new on-line sample injection device for the liquefied gas mixture in liquid or gas state, and applied to the analysis of liquefied gas mixture of ethylene oxide and fluorinated hydrocarbons by GC/AED (gas chromatograph-atomic emission detector). We studied performance of AED, and effect of sample introduction and selected wavelength to the accuracy and repeatability of analytical results.

Pectinase-treated Panax ginseng ameliorates hydrogen peroxide-induced oxidative stress in GC-2 sperm cells and modulates testicular gene expression in aged rats

  • Kopalli, Spandana Rajendra;Cha, Kyu-Min;Jeong, Min-Sik;Lee, Sang-Ho;Sung, Jong-Hwan;Seo, Seok-Kyo;Kim, Si-Kwan
    • Journal of Ginseng Research
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    • v.40 no.2
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    • pp.185-195
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    • 2016
  • Background: To investigate the effect of pectinase-treated Panax ginseng (GINST) in cellular and male subfertility animal models. Methods: Hydrogen peroxide ($H_2O_2$)-induced mouse spermatocyte GC-2spd cells were used as an in vitro model. Cell viability was measured using MTT assay. For the in vivo study, GINST (200 mg/kg) mixed with a regular pellet diet was administered orally for 4 mo, and the changes in the mRNA and protein expression level of antioxidative and spermatogenic genes in young and aged control rats were compared using real-time reverse transcription polymerase chain reaction and western blotting. Results: GINST treatment ($50{\mu}g/mL$, $100{\mu}g/mL$, and $200{\mu}g/mL$) significantly (p < 0.05) inhibited the $H_2O_2$-induced ($200{\mu}M$) cytotoxicity in GC-2spd cells. Furthermore, GINST ($50{\mu}g/mL$ and $100{\mu}g/mL$) significantly (p < 0.05) ameliorated the $H_2O_2$-induced decrease in the expression level of antioxidant enzymes (peroxiredoxin 3 and 4, glutathione S-transferase m5, and glutathione peroxidase 4), spermatogenesis-related protein such as inhibin-${\alpha}$, and specific sex hormone receptors (androgen receptor, luteinizing hormone receptor, and follicle-stimulating hormone receptor) in GC-2spd cells. Similarly, the altered expression level of the above mentioned genes and of spermatogenesis-related nectin-2 and cAMP response element-binding protein in aged rat testes was ameliorated with GINST (200 mg/kg) treatment. Taken together, GINST attenuated $H_2O_2$-induced oxidative stress in GC-2 cells and modulated the expression of antioxidant-related genes and of spermatogenic-related proteins and sex hormone receptors in aged rats. Conclusion: GINST may be a potential natural agent for the protection against or treatment of oxidative stress-induced male subfertility and aging-induced male subfertility.

Aroma Characterization of Roasted Bulgogi Reaction Flavor Manufactured by a High-temperature Reaction Apparatus (고온반응기로 제조한 구운 불고기 반응향의 향미특성)

  • Seo, Won-Ho;Kim, Young-Kwon;Jang, Seong-Ho;Baek, Hyung Hee
    • Korean Journal of Food Science and Technology
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    • v.47 no.2
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    • pp.176-183
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    • 2015
  • To characterize the aroma properties of roasted bulgogi reaction flavor obtained by using a high-temperature reaction apparatus, the volatile flavor and aroma-active compounds were analyzed using simultaneous steam distillation and solvent extraction (SDE)-gas chromatography-mass spectrometry-olfactometry (GC-MS-O). One hundred five volatile compounds were detected in roasted bulgogi reaction flavor using GC-MS. Out of these compounds, furfural was the most abundant volatile compound, followed in order of abundance by 5-methyl furfural, phenylacetaldehyde, and nonanal. Of the volatile compounds identified in roasted bulgogi reaction flavor, 33 aroma-active compounds were detected using GC-O. 2,3-Butanedione and furfural were the most intense aroma-active compounds detected. Other relatively intense odorants included hexanal, octanal, nonanal, undecanal, phenylacetaldehyde, 5-methyl furfural, 2,6-dimethyl pyrazine, and dimethyl trisulfide. These were important aroma-active compounds that contributed to the aroma of roasted bulgogi reaction flavor because of their potency and aroma properties. The concentrations of the aroma-active compounds increased as the reaction temperature increased, whereas those of the sulfide compounds decreased.

A Rapid Method for Analysing Polycyclic Aromatic Hydrocarbons (PAH's) in Urban Dust Using Supercritical Fluid Extraction (SFE) and Gas Chromatography/Mass Spectrometry (GC/MS)허귀석, 김달호 (초임계유체추출과 GC/MS를 이용한 도심 대기분진 중 PAH들의 신속한 분석법에 관한 연구)

  • Heo, Gwi Seok;Kim, Dal Ho
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.726-733
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    • 1994
  • Supercritical fluid extraction (SFE) followed by gas chromatographic separation and mass spectrometric (MS) detection were used in rapid analysis of polycyclic aromatic hydrocarbons (PAH's) in air particulate material extracted for 30 min with 10 ml of supercritical $N_2O$ without another sample preparation step. Two samples, urban dust in Seoul area and a certified air particulate reference material 1649 supplied by the NBS (National Bureau of Standards), were processed for the purpose of evaluating extraction and analysis methods. As a result, the quantitative recovery of PAH's in the SFE method was relatively lower than conventional organic solvent extraction methods, but reproducibility was resonable, and analysis time was reduced remarkably. The method has proved to be suitable for monitoring of PAH's in air particulate material.

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Characterization of the Aroma of Salt-fermented Anchovy Sauce Using Solid Phase Microextraction-Gas Chromatography-Olfactometry Based on Sample Dilution Analysis

  • Kim, Hyung-Joo;Baek, Hyung-Hee
    • Food Science and Biotechnology
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    • v.14 no.2
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    • pp.238-241
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    • 2005
  • Aroma-active compounds were evaluated from salt-fermented anchovy sauce by solid phase microextraction-gas chromatography-olfactometry (SPME-GC-O) based on sample dilution analysis (SDA). SPME extract from carboxen/polydimethylsiloxane (CAR/PDMS) fiber was the most similar to the original odor of salt-fermented anchovy sauce used for this experiment, followed by divinylbenzene/CAR/PDMS (DVB/CAR/PDMS) fiber. Because salt-fermented anchovy sauce contains 23% NaCl, NaCl concentration of diluent was considered when salt-fermented anchovy sauce was serially diluted. Linear relationship between GC response and sample concentration was observed when diluted with 23% NaCl solution, whereas not observed when diluted with deodorized distilled water. Eleven and 16 aroma-active compounds were detected by SPME-GC-O based on SDA using CAR/PDMS and DVB/CAR/PDMS fibers, respectively. Butanoic acid and 3-methyl butanoic acid showed the highest ${\log}_2SD$ factors for CAR/PDMS and DVB/CAR/PDMS fibers. Dimethyl trisulfide, methional, trimethyl amine, 1-penten-3-ol, and acetic acid were also detected as potent aroma-active compounds.

GC-MS Analysis of Amur Cork Tree Extract and Its Degradation Products

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.34 no.6
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    • pp.1042-1052
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    • 2010
  • The Degradation of amur cork tree extract is investigated by GC-MS after treating the dye with three thermal degradation systems of, room temperature (RT), $4^{\circ}C$ refrigeration (LT), $100^{\circ}C$ oven (OV), and $H_2O_2$/UV/$O_2$ (PER) degradation system for 0-24 days. It was found that PER degradation system represented the highest intensity of degradation treatment followed by OV treatment among the four degradation parameters. The possible fingerprint products of amur cork tree dye, that yielded 68% (or higher) reliability in the NIST spectral match, were isobenzofuran-1,3-dione,4,5-dimethoxy- (8.37 min, PER only), 1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro (9.41 min, PER only), canthine-6-one (10.24 min, RT, LT, OV only), and dihydroberberine (15.05 min, RT, LT, OV, PER) in the order of higher to lower possibility of detection. Unknown products 7 (13.43 min) and 8 (16.35 min) are two other possible fingerprint products of amur cork tree dye that require future identification.