• Title/Summary/Keyword: gas chromatography/mass spectrometry (GC/MS)

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

  • Kim, Yong-Yeon;Shin, Han-Seung
    • Food Science and Industry
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    • v.55 no.1
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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.

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

  • Choi, Hae-Min;Yum, Tae-Woo;Paeng, Gi-Jeong;Kim, Yun-Je
    • Analytical Science and Technology
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    • v.24 no.3
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    • pp.183-192
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    • 2011
  • This study was done for the determination and excretion profile of superdrol and its metabolites in human urine using both liquid chromatography with electrospray ionization mass spectrometry and gas chromatography with mass spectrometry after trimethylsilylation. Superdrol and its two metabolites were detected in human urine after administration of superdrol to healthy volunteers. The intra-day recovery ranged 89.7-113.2%, accuracy ranged 91.8-113.8% and reproducibility ranged 0.2-6.8% and inter-day recovery ranged 89.3-104.1%, accuracy ranged 95.2-103.0%, reproducibility ranged 0.7-7.8%. We found that superdrol M1 was a hydration at C-3 and superdrol M2 was a hydroxylation at D-ring. Superdrol and two metabolites were excreted as their glucuronided fractions. The glucuro-/sulfa-conjugated ratio of superdrol, superdrol M1 and superdrol M2 were 0.02, 0.02, 0.01, respectively. The excretion studies showed that superdrol and two metabolites were reached 4.3 h after oral administration and superdrol and superdrol M1 were detected until 48 h in human urine.

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

  • Yoon, Hye-Ran
    • Journal of The Korean Society of Inherited Metabolic disease
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    • v.6 no.1
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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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    • v.30 no.2
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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
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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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.

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

  • Shin, Seong-Kee;Kim, Sang-Ho;Lee, Yoon-Hyung;Rhee, Kyu-Soon
    • Korean Journal of Food Science and Technology
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    • v.24 no.1
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    • pp.25-28
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    • 1992
  • The changes of amount in flavor components of chewing gum during storage of various relative humidity were studied by GC/MS. The volatile components in chewing gum were extracted by sample preperation and 15 volatile components were identified by NIST/NBS library searching. According to the period of storage, quantities of major volatile components extracted by tetrahydrofuran-methanol solutions were determined by using tetradecane as internal standard. Until 4 weeks, comparing with starting peak area ratio, the decrease of chewing gum flavor components were rapid at 33, 75 than 53 R.H(%). And after 16 weeks, amount of chewing gum flavor at all storage conditions similarly decreased to $45{\sim}49%$ of the initial amount.

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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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    • v.26 no.2
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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.

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

  • Yoo, Eun-Ah;Park, Do-Yeon;Lee, Hyang-Ki;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.221-228
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    • 2002
  • AMX is one of extremely high mutagenic compound produced from the reaction of the chlorine and the organic compound during the disinfection of tap water. In this paper, the chemical derivatization of MX with 2% sulfuric acid-methanol, iso-propanol, sec-butanol and n-butanol derivatives for the GC/MS analysis were tested or compared. Limit of detection for the EI and NCI mode were 25 pg and 1.25 pg, respectively. The good linear calibration curve was obtained the range of 25~2500 pg by EI and NCI

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

  • Kim, Jin-Young;Kim, Jong-Sang;Kim, Min-Kyoung;Lee, Jae-Il;Suh, Yong-Jun;In, Moon-kyo
    • YAKHAK HOEJI
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    • v.51 no.3
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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%.

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

  • Park, Hyun-Mee;Kim, Young-Man;Lee, Dai-Woon;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.471-475
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    • 2001
  • Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

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