• 제목/요약/키워드: gas chromatography mass spectrometry

검색결과 989건 처리시간 0.022초

Determination of Persistent Organochlorine Pollutants in Rat Hair by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Pyo, Hee-Soo;Park, Song-Ja
    • Bulletin of the Korean Chemical Society
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    • 제25권10호
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    • pp.1489-1494
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    • 2004
  • A gas chromatography/mass spectrometric assay method was developed for the determination of persistent organochlorine pollutants (POPs) in hair. For the exact extraction study was used hair of rat exposed with POPs. Sonication of the hair matrix with 3 M HCl solution in methylene chloride of the extraction methods studied was the most efficient and rapid sample preparation method. After sonication of rat hair was achieved clean up with a solid phase extraction procedure using silica gel-florisil. Elution was performed with 8 mL of methylene chloride. The eluate was concentrated to approximately 100 ${\mu}L$ and analyzed by gas chromatography-mass spectrometry (GC-MS). Detection limits of POPs were in the concentration range of 0.6-1.2 ng/g in rat hair. Aldrin, dieldrin, p,p-DDT and mirex were dosed rat for 4 weeks at concentration of 0.01 mg/L in drinking water and detected in rat hair at concentration of 2.8, 11.3, 7.9 and 15.6 ng/g, respectively. Aldrin and p,p-DDT were metabolized to dieldrin and p,p-DDE, which were detected in concentration of 9.7 and 2.9 ng/g in rat hair, respectively. The developed method may be valuable to be used to analyze POPs in human hair.

Enantioseparation of Flurbiprofen and Ketoprofen in Patches and in Urine Excretions by Achiral Gas Chromatography

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Kim , Kyoung-Rae
    • Archives of Pharmacal Research
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    • 제27권12호
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    • pp.1295-1301
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    • 2004
  • The enantiomeric composition tests on flurbiprofen and ketoprofen present in patch products and in urine excretions following patch applications were performed as diastereomeric (R)-(+)- 1-phenylethylamides by achiral gas chromatography and by gas chromatography-mass spectrometry in selected ion monitoring mode. The method for determination of (R)- and (S)-enantiomers in the range from 0.1 to 5.0 ${\mu}$g was linear (r ${\ge}$ 0.9996) with acceptable precision (% RSD ${\le}$5.2) and accuracy (% RE = 0.6 ~ -2.4). The enantiomeric compositions of flurbiprofen in one patch product and of ketoprofen in five different products were identified to be racemic with relatively good precision (${\le}$ 6.4%). The urinary excretion level of (R)-flurbiprofen was two times higher than its antipode, while the comparable excretion levels of (R)- and (S)-enantiomers for ketoprofen were observed.

Separation of Light Rare-Earth Elements Using Gas-Pressurized Extraction Chromatography

  • Kim, Namuk;Park, Jai Il;Um, Wooyong;Kim, Jihye
    • Mass Spectrometry Letters
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    • 제12권4호
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    • pp.186-191
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    • 2021
  • A new method for chemical separation of light rare-earth elements (LREEs) using gas-pressurized extraction chromatography (GPEC) is described. GPEC is a microscale column chromatography system that features a constant flow of solvents, which is created by pressurized nitrogen gas. The separation column with a Teflon tubing was packed with LN resin. The proposed GPEC method facilitates production of lesser chemical wastes and faster separation owing to the use of low solvent volume compared to traditional column chromatography. We evaluated the separation of Ba, La, Ce, and Nd using various elution solvents. The column reproducibility of the proposed GPEC system ranged from 2.4% to 4.9% with RSDs of recoveries, and the column-to-column reproducibility ranged from 3.1% to 6.3% with RSDs of recoveries. The proposed technique is robust, and it can be useful for the fast separation of LREEs.

Liquid Chromatography-Mass/Mass Spectrometry (MS)와 Gas Chromatography-MS를 이용한 농축 액상 비료제품 중 Indole-3-acetic acid 및 Indole-3-butyric acid 정량분석능 비교 (Comparison of Liquid Chromatography-Mass/Mass Spectrometry (MS) and Gas Chromatography-MS for Quantitative Analysis of Indole-3-acetic acid and Indole-3-butyric acid from the Concentrated Liquid Fertilizer)

  • 김진효;박종민;최근형;박연기;임건재;김두호;권오경
    • Journal of Applied Biological Chemistry
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    • 제56권1호
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    • pp.53-57
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    • 2013
  • 비료제품에는 의도적 혹은 비의도적으로 농약으로 등록된 indole-3-acetic acid (IAA) 및 indole-3-butyric acid (IBA)성분에 대한 잔류 가능성이 꾸준히 제기되고 있으나, 생장조정제가 아닌 비료제품에서 mg/L 수준의 옥신류 잔류분석법이 마련되어 있지 않았다. 따라서, 본 연구에서는 생체시료에 미량 잔류하는 IAA 및 IBA 분석에 사용되어 온 liquid chromatography-mass/mass spectrometry (LC-MS/MS)와 gas chromatography-MS 기기분석법을 활용하여 농축 액상비료제품에 적용할 수 있는지 조사하였으며, 액상 비료제품에 적용 가능한 정밀기기 분석법을 개발하고자 하였다. 수용액 상태의 시료에서 식물 생장호르몬인 IAA와 IBA를 가장 손쉽게 정제할 수 있는 방법으로 hydrophile-lipophile balance (HLB) solid phase extraction를 활용하였으나, 제한된 조건에서 LC-MS/MS를 통한 정량분석은 적합한 회수율을 확보하지 못하였고, 정성분석만 가능함을 확인하였다. 반면, 비료제품 250배 희석액을 사용하여 HLB 정제, trimethylsilyl chloride을 이용한 methylation을 통한 GC-MS 분석에서는 검출한계 1.4 mg/L과 93-107%의 회수율로 액상 비료제품에서 IAA와 IBA 정량분석법을 확립할 수 있었다.

GC-MS Analysis of Ricinus communis, Pongamia pinnata, Datura metal, Azadirachta indica, Acalypha indica (leaf) Extract Using Methanol Extraction

  • J. Varshini premakumari;M. Job Gopinath
    • Mass Spectrometry Letters
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    • 제14권3호
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    • pp.79-90
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    • 2023
  • Natural goods, especially therapeutic plants, are abundant in the World. Because they have the ability to provide all humanity with countless advantages as a source of medicines, medicinal plants are presently receiving more attention than ever. These plants' therapeutic efficacy is based on bioactive phytochemical components that have clear physiological effects on the human body. The drying process is crucial for the preparation of plant materials prior to extraction since freshly harvested plant materials include active enzymes that create active components, intermediates, and metabolic processes. Many of the phytoconstituents may be extracted using the semi-polar solvent methanol. The goal of the current work is to use the GC-MS gas chromatography- mass spectrometry technology to identify the phytochemicals and review their biological activity. In methanol leaf extract, 5 phytocompounds were found in Ricinus communis, 5 phytocompounds in Pongamia pinnata, 12 phytocompounds in Datura metal, 7 phytocompounds in Azadirachta indica, 11 phytocompounds in Acalypha indica.

GC-MS and GC-FID Analysis of Citronella Oil Products for Indicator Ingredient Identification

  • Sumin Kang;Wooil Kim;Jin Wuk Lee;Sangwon Cha
    • Mass Spectrometry Letters
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    • 제14권4호
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    • pp.160-165
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    • 2023
  • Citronella oil, an essential oil extracted through steam distillation from the leaves and stems of Cymbopogon, is a natural complex substance (NCS) regulated by the Korean government for its use in insect repellents. The component ratios of NCSs like citronella oil vary due to differences in manufacturing processes and origins, presenting a challenge in identifying and quantifying these substances in consumer chemical products. This study analysed ten commercially available products of the most commonly used types of citronella oil, specifically Java and Ceylon types, using gas chromatography (GC)-mass spectrometry (MS) and GC with flame ionization detection (FID). Through chromatographic data, we aimed to determine the components that can qualitatively identify citronella oil and the indicator ingredients that can be used for content analysis.

Determination of more than 500 Pesticide Residues in Hen Eggs by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) and Gas Chromatography-Tandem Mass Spectrometry (GC/MS/MS)

  • Golge, Ozgur;Liman, Turan;Kabak, Bulent
    • 한국축산식품학회지
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    • 제41권5호
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    • pp.816-825
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    • 2021
  • This study aims to validate a fast method of simultaneous analysis of 365 LCamenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 ㎍/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 ㎍/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.

Comparison of the Fatty Acid Composition and Small Molecular Metabolites between Yanjin Blackbone Chicken and Piao Chicken Meat

  • Rong Jia;Wen Xun;Guozhou Liao;Yuan Yang;Guiying Wang
    • 한국축산식품학회지
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    • 제43권6호
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    • pp.975-988
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    • 2023
  • The fatty acid composition and small molecular metabolites in breast and leg meat of Yanjin blackbone chickens (YBC) and Piao chickens (PC) were detected by gas chromatography-mass spectrometry and liquid chromatography-quadrupole static field orbital trap mass spectrometry. Thirty-two fatty acids were detected, and the total fatty acid content of PC was significantly higher than that of YBC (p<0.05). Oleic acid, linoleic acid, palmitic acid, stearic acid, and arachidonic acid were the main fatty acids in the two chicken varieties, and the composition of fatty acids in the two varieties were mainly unsaturated fatty acids, being more than 61.10% of the total fatty acids. Meanwhile, 12 and 16 compounds were screened out from chicken legs and chicken breasts of YBC and PC, respectively, which had important contributions to the differences between groups.

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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    • 제23권4호
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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.

Gas Chromatography-mass Spectrometry와 Headspace-Gas Chromatography-mass Spectrometry를 이용한 제주산 민트 에센셜오일 성분 분석 (Analysis of Mint Essential Oils from Jeju Island, Korea by Gas Chromatography-mass Spectrometry and Headspace-Gas Chromatography-mass Spectrometry)

  • 현호봉;부경환;강혜림;김소미
    • Journal of Applied Biological Chemistry
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    • 제58권2호
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    • pp.175-181
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    • 2015
  • 제주에서 생산된 페퍼민트, 스피아민트, 오데코롱민트 3종으로 부터 추출한 에센셜오일의 성분을 기체 크로마토그래피-질량분석기(GC-MS)와 headspace-GC-MS (HS-GC-MS)를 이용하여 분석하였다. GC-MS 분석결과 페퍼민트, 스피아민트, 오데코롱민트 각각에서 13종의 성분이 동정되었다. 전체 이온 크로마토그램의 피크 intensity를 기초로 보았을 때, 페퍼민트에서는 peperitenone oxide, 스피아민트에서는 carvone과 limonene, 오데코롱민트에서는 linalool이 주 화합물로 동정되었다. HS-GC-MS 분석에서는 GC-MS와 비교하였을 때 alcohol과 acetate와 같은 휘발성이 강한 성분이 많이 검출되었고, 검출되는 성분의 수도 증가하였다. 하지만 스피아민트와 오데코롱민트의 주 화합물은 GC-MS에서 검출된 것과 같았고, 페퍼민트에서만 GC-MS에서 낮은 함량을 보였던 menthol이 주요화합물로 동정되었다. 흥미롭게도, 오데코롱민트 에센셜 오일에서 linalyl acetate와 linalool의 함량이 탁월하게 높음을 확인했다.