• 제목/요약/키워드: Gas chromatography/mass spectrometry (GC/MS)

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식품 중 다환방향족탄화수소 분석법 연구 (A study on analytical methods for polycyclic aromatic hydrocarbons in foods)

  • 김용연;신한승
    • 식품과학과 산업
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    • 제55권1호
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    • pp.45-57
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    • 2022
  • This study was proceeded the analytical methods using various analytical instruments for polycyclic aromatic hydrocarbons (PAHs) in food products. Various analytical methods were developed to determine levels of PAHs including benzo[a]pyrene, benzo[a]anthracene, benzo[b]fluoranthene, and chrysene formed in various food products using gas chromatography-mass spectrometry (GC-MS), enzyme-linked immunosorbent assay (ELISA) and raman spectroscopy. Recently, the rapid on-site response for the detection of hazardous substances in food aims to develop an onsite rapid detection of a simplified technical analysis method to reduce the time and cost required for analysis of PAHs. Current PAHs detection methods have been reviewed along with new raman spectroscopy analytical method.

LC/TOF-MS와 GC/TOF-MS를 이용한 인체 내 요시료 중 Superdrol과 그 대사체의 분석 (Determination of superdrol and its metabolites in human urine by LC/TOF-MS and GC/TOF-MS)

  • 최해민;염태우;팽기정;김연제
    • 분석과학
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    • 제24권3호
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    • pp.183-192
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    • 2011
  • 본 연구에서는 LC/ESI/MS 및 GC/MS로 superdrol을 인체에 경구투여 한 후 채취한 요시료 중에 함유된 superdrol 및 그 대사체의 분석법을 확립하고 이들의 체내 배설형태를 조사하였다. 액체-액체 추출에서 최적 추출 pH는 6.5 이고 최적 추출 용매는 diethly ether이였다. GC/MSD를 이용하여 superdrol과 그 대사체의 분석법에 대한 유효성을 점검한 결과, intra-day의 회수율은 89.7-113.2%, 정확도 91.8-113.8%, 재현성은 0.2-6.8%로 나타났고 inter-day의 회수율은 89.3-104.1%, 정확도는 95.2-103.0%, 재현성은 0.7-7.8%로 나타났다. LC/ESI/MS을 통해 얻은 blank urine과 dosed urine의 크로마토그램을 비교하여 superdrol의 대사체를 검출하였으며 Superdrol과 그 대사체를 유도체화 시켜 GC/TOF-MS로 확인하였다. 확보된 질량스펙트럼으로부터 superdrol M1의 경우 superdrol의 3-C 위치의 케톤기가 하이드록시기로 환원된 것으로 추정할 수 있었고 M2의 경우 superdrol의 D-ring에 하이드록시기가 첨가된 것으로 추정할 수 있었다. 또한, 효소가수분해과정을 비교해 본 결과 superdrol과 그 대사체들은 대부분 글루쿠론산 포합체를 형성하여 체외로 배설되는 것을 확인하였다. Superdrol 경구투여 후 채취한 요시료로부터 superdrol과 그 대사체의 배설양상을 조사한 결과, 모두 4.3 시간에서 최대배설량을 보였고 superdrol과 superdrol M1은 48시간까지도 미량검출 되어 체내 잔류성이 높은 물질임을 확인할 수 있었다.

GC-MS 크로마토그램의 컴퓨터 자동해석을 이용한 유전성 대사질환의 진단법 개발 (Development of a GC-MS Diagnostic Method with Computer-aided Automatic Interpretation for Metabolic Disorders)

  • 윤례란
    • 대한유전성대사질환학회지
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    • 제6권1호
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    • pp.40-51
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    • 2006
  • Purpose: A personal computer-based system was developed for automated metabolic profiling of organic aciduria and aminoacidopathy by gas chromatography-mass spectrometry and data interpretation for the diagnosis of metabolic disorders Methods: For automatic data profiling and interpretation, we compiled retention time, two target ions and their intensity ratio for 77 organic acids and 13 amino acids metabolites. Metabolites above the cut-off values were flagged as abnormal compounds. The data interpretation was a based on combination of flagged metabolites. Diagnostic or index metabolites were categorized into three groups, "and", "or" and "NO" compiled for each disorder to improve the specificity of the diagnosis. Groups "and" and "or" comprised essential and optional compounds, respectively, to reach a specific diagnosis. Group "NO" comprised metabolites that must be absent to make a definite diagnosis. We tested this system by analyzing patients with confirmed Propionic aciduria and others. Results: In all cases, the diagnostic metabolites were identified and correct diagnosis was founded to be made among the possible disease suggested by the system. Conclusion: The study showed that the developed method could be the method of choices in rapid, sensitive and simultaneous screening for organic aciduria and amino acidopathy with this simplified automated system.

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Analysis of Minor Additives and Polymer in Used-stripper Using Pyrolysis-Gas Chromatography/Mass Spectrometry and Electrospray Mass Spectrometry

  • Koo, Jeong-Boon;Park, Chang-Hyun;Han, Cheol;Na, Yun-Cheol
    • Bulletin of the Korean Chemical Society
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    • 제30권2호
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    • pp.368-372
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    • 2009
  • The trace polymer and additives in used stripper solutions were analyzed by a combination of Py-GC/MS and ESI-MS. In the comparison of the pyrolysates produced by the pyrolysis of the pure stripper and photoresist at $500{^{\circ}C}$, the presence of novolac polymer in the used stripper was confirmed by the presence of the characteristic peaks of its pyrolysates, such as those of the methylphenol, di-methylphenol and methylenebis(methylphenol) isomers. The intact trace polymer was measured by ESI-MS, which showed the distribution of oligomers at intervals of 120 Da, indicating di-methylphenol to be the repeat unit. Additional MS/MS measurements demonstrated that the end group is methylphenol and the repeat groups are di-methylphenol. Some modified oligomers caused by the methylation or di-methylation of the repeat unit were also identified. Although the polymer is only present at a trace level in the used stripper, these combined analytical methods provided the means to qualify the stripper solution through the identification and structural determination of the polymer.

Determination of agrochemical residues in tobacco using matrix solid-phase dispersion and GC/MS

  • Lee, Jeong-Min;Min, Hye-Jeong;Park, Jin-Won;Lee, Moon-Young;Jang, Gi-Chul
    • 한국연초학회지
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    • 제36권1호
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    • pp.12-19
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    • 2014
  • A matrix solid-phase dispersion (MSPD) method was developed for extracting and cleaning-up the selected agrochemicals in tobacco using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS-SIM). Different parameters of the method were investigated and optimized, such as the type of solid-phase (alumina, $C_{18}$ and Florisil) and eluent (acetone, acetonitrile, ethylacetate and n-hexane). The best results were obtained using 0.5 g of tobacco sample, 1.0 g of $C_{18}$ as dispersant sorbent, 1.0 g of Florisil as clean-up sorbent and acetonitile saturated with n-hexane as eluting solvent. The method was validated using tobacco samples fortified with agrochemicals at their different concentration levels. This method gave good linearity for the selected agrochemicals of ranging from $0.01{\mu}g/mL$ to $0.1{\mu}g/mL$. Recoveries of the selected agrochemicals in tobacco were more than 80 % and reproducibilities were found to be better than 10 % RSD. Those results suggested that the analytical procedure including MSPD method in combining with GC/MS could be applicable to the rapid determination often the selected agrochemicals in tobacco.

GC/MS에 의한 저장중 츄잉껌 향기성분 변화연구 (Changes of Flavor Components in Chewing Gum during Storage by Gas Chromatography/Mass Spectrometry)

  • 신성기;김상호;이윤형;이규순
    • 한국식품과학회지
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    • 제24권1호
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    • pp.25-28
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    • 1992
  • 츄잉껌 품질향상의 일환으로 저장기간 및 여러 가지 상대습도하에서 츄잉껌 향기성분의 변화를 GC/MS로 분석하였다. 츄잉껌 향기성분을 시료전처리로 포집하고 tetradecane을 내부표준용액으로 이용해서 각 성분과의 peak area ratio로써 향기성분함량의 감소량을 측정한 결과 저장초기에는 53% R.H 저장분 보다 33, 75% R.H에서 감소속도가 빨라으나 그 이후는 차이가 별로 없었으며 16주 후에는 $45{\sim}49%$의 잔존량을 나타내었다.

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Butyrylcholinesterase Inhibitory Activity and GC-MS Analysis of Carica papaya Leaves

  • Khaw, Kooi-Yeong;Chear, Nelson Jeng Yeou;Maran, Sathiya;Yeong, Keng Yoon;Ong, Yong Sze;Goh, Bey Hing
    • Natural Product Sciences
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    • 제26권2호
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    • pp.165-170
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    • 2020
  • Carica papaya is a medicinal and fruit plant owing biological activities including antioxidant, antiviral, antibacterial and anticancer. The present study aims to investigate the acetyl (AChE) and butyryl (BChE) cholinesterase inhibitory potentials of C. papaya extracts as well as their chemical compositions. The chemical composition of the active extract was identified using a gas chromatography-mass spectrometry (GC-MS). Ellman enzyme inhibition assay showed that the alkaloid-enriched leaf extract of C. papaya possessed significant anti-BChE activity with an enzyme inhibition of 75.9%. GC-MS analysis showed that the alkaloid extract composed mainly the carpaine (64.9%) - a major papaya alkaloid, and some minor constituents such as aliphatic hydrocarbons, terpenes and phenolics. Molecular docking of carpaine revealed that this molecule formed hydrogen bond and hydrophobic interactions with choline binding site and acyl pocket. This study provides some preliminary findings on the potential use of C. papaya leaf as an herbal supplement for the prevention and treatment of Alzheimer's disease.

GC/MS를 이용한 MX 유도체화 분석법 연구 (Analysis of derivatized MX by Gas Chromatography/Mass Spectrometry)

  • 유은아;박도연;이향기;명승운
    • 분석과학
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    • 제15권3호
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    • pp.221-228
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    • 2002
  • MX [3-chloro-4(dichloromethyl)-5-hydroxy-2(5H)-furanone]는 수돗물의 소독을 위해 첨가한 염소와 수중의 유기물이 반응하여 생성되는 강력한 변이원성 물질이다. 본 논문에서는 GC/MS를 이용하여 유도체화 시약인 2% 황산-methanol, iso-propanol, sec-butanol, n-butanol을 이용하여 MX의 유도체화를 비교하였으며, 이온화 방법으로 EI 와 NCI를 비교한 결과, NCI 방법에서 검출 한계가 1.25 pg으로 EI 방법에서는 25 pg이였으며, 25~2500 pg 범위에서 직선성을 나타내었다.

GC/MS를 이용한 모발 중 메스암페타민 및 암페타민 분석의 측정불확도 평가 (Uncertainty Evaluation of the Analysis of Methamphetamine and Amphetamine in Human Hair by GC/MS)

  • 김진영;김종상;김민경;이재일;서용준;인문교
    • 약학회지
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    • 제51권3호
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    • pp.206-213
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    • 2007
  • Recently estimating the uncertainty of an analytical result has become an essential part of quantitative analysis. This study describes the uncertainty of the measurement for the determination of methamphetamine and its major metabolite amphetamine in human hair, The method consists of washing, drying, weighing, incubation and extraction with methanolic HCI solution, clean-up, trifluoroacetyl derivatization, and qualification/quantification of residues by gas chromatography/mass spectrometry (GC/MS). Traceability of measurement was established through traceable standards and calibrated volumetric equipment and measuring instruments. Measurement uncertainty associated with each analyte in real samples was estimated using quality control (QC) data. The main source of combined standard uncertainty comprised two components, which are uncertainties associated with calibration linearity and variations in QC, while those associated with preparation of analytical standards and sample weighing were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method ranged for individual analytes from 4.99 to5.03%.

SPME-GC-MS를 이용한 DBCP 및 n-Butylbenzene의 분석 (Determination of DBCP and n-Butylbenzene using SPME with GC-MS)

  • 박현미;김영만;이대운;이강봉
    • 분석과학
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    • 제14권6호
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    • pp.471-475
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    • 2001
  • $85{\mu}m$-polyacrylate(PA) 와 $100{\mu}m$-polydimethylsiloxane(PDMS) fiber를 사용하여 물증의 DBCP와 n-butylbenzene을 추출한 후 GC-MS로 분석하는 방법을 연구하였다. SPME 과정에 영향을 미치는 인자들, 즉 추출 시간, 주입 길이, 주입 온도, 탈착 시간 및 탈착 온도들에 대한 최적화 조건을 조사하였다. 검량선의 직선성(correlation coefficient, R)은 0.99 이상이었으며, 본 분석법의 검출한계는 1.5 와 $10.8{\mu}g/L$ 이었고, 분석법의 재현성은 RSD 10.4와 14.4 % 였다.

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