• Title/Summary/Keyword: gas chromatograph-mass spectrometry

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Identification of Coffee Fragrances Using Needle Trap Device-Gas Chromatograph/Mass Spectrometry (NTD-GC/MS)

  • Eom, In-Yong;Jung, Min-Ji
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1703-1707
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    • 2013
  • A fast and simple sampling and sample preparation device, (NTD) has been developed and applied to sample and analyze volatile components from ground coffee beans. Coffee fragrances and other volatile organic compounds (VOCs) were sampled by the NTD and then analyzed by gas chromatograph-mass spectrometry (GC/MS). Divinylbenzene (DVB) particles (80/100 mesh size) were the sorbent bed of the NTD. More than 150 volatile components were first identified based on the database of the mass library and then finally 30 fragrances including caffeine were further confirmed by comparing experimental retention indices (i.e. Kovat index) with literature retention indices. Total sampling time was 10 minutes and no extra solvent extraction and/or reconstitution step need. Straight n-alkanes (C6-C20) were used as retention index probes for the calculation of experimental retention indices. In addition, this report suggests that an empty needle can be an alternative platform for analyzing polymers by pyrolysis-GC/MS.

Determination of Organophosphorous Pesticides in Suncheon Bay (순천만 유기인제제 농약의 측정)

  • JEON, DEOK SAN;YANG, JAE SAM
    • 한국해양학회지
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    • v.25 no.1
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    • pp.21-25
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    • 1990
  • Eleven water samples were analyzed for organophosphorous pesticides in Suncheon Bay with Gas Chromatography Mass Spectrometry. For the first time in Korea, Kitazin-P was found in marine environment and the concentrations ranged upto 2.2mg/l. The regional and temporal variations of the pesticide were also studied.

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Insecticidal Activity of Spearmint Oil against Trialeurodes vaporariorum and Bemisia tabaci Adults (온실가루이와 담배가루이에 대한 Spearmint Oil의 살충활성)

  • Choi Yu-Mi;Kim Gil-Hah
    • Korean journal of applied entomology
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    • v.43 no.4 s.137
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    • pp.323-328
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    • 2004
  • These studies were carried out to investigate the fumigation and contact toxicities of spearmint oil (Mentha spicata) against adults of greenhouse whitefly, Trialeurodes vaporariorum and sweet-potato whitefly, Bemisia tabaci. And we carried out the constituent analysis of spearmint oil using gas chromatograph (GC) and gas chromatograph mass spectrometry (GC/MS). Spearmint oil showed $99.1\%,\;91.7\%,\;41.1\%$ fumigation toxicity against T. vaporariorum adults at $10{\mu}L/954mL,\;5{\mu}L/954mL,\;1{\mu}L/954mL$ air concentration, respectively. In case of B. tabaci adults, spearmint oil showed $100\%,\;100\%,\;61.3\%$ fumigation toxicity, respectively. However, spearmint oil showed < $30\%$ contact toxicity against adults of T. vaporariorum and B. tabaci. Through the constituent analysis using GC and GC/MS, we confirmed main constituents of spearmint oil were limonene ($16.1\%$), ${\gamma}$-terpinene($13.8\%$), ${\rho}$-cymene($5.8\%$), 3-octanol($6.9\%$), carvone($40.9\%$). Carvone, major constituent of spearmint oil, also showed $100\%$ fumigation toxicity at $10{\mu}L/954mL$ air concentration.

Simultaneous Analysis of Several Non-Steroidal Anti-Inflammatory Drugs in Urine by Gas Chromatograph/Negative Chemical Ionization-Mass Spectrometry (기체 크로마토그래프-질량분석법을 이용한 뇨중 비스테로이드성 소염진통제 (NSAIDs)의 동시 분석법)

  • Myung, Seung-Woon;Park, Joon-Ho;Kim, Myung-Soo;Cho, Hyun-Woo
    • Analytical Science and Technology
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    • v.12 no.6
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    • pp.571-576
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    • 1999
  • Screening method for NSAIDs (Hon-Steroidal Anti-Inflammatory Drugs) in urine was developed using GC/NCI-MS. Derivatized six fenamates with pentafluoropropionic anhydride showed high sensitivity in NCI-MS. The conditions of the derivatization reaction and chromatographic conditions were established for screening with a trace analysis. Limit of detection was in the range of 4-25 pg/mL. This method may be used to the equine doping analysis for NSAIDs and forensic analysis.

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Analysis of Volatile Compounds and Enantiomeric Separation of Chiral Compounds of Dried Sancho (Zanthoxylum schinifolium Siebold & Zucc)

  • Seo, Hye-Young;Shim, Sung-Lye;Ryu, Keun-Young;Jung, Min-Seok;Hwang, In-Min;Shin, Dong-Bin;Kwon, Joong-Ho;Schreier, Peter;Kim, Kyong-Su
    • Food Science and Biotechnology
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    • v.18 no.1
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    • pp.18-24
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    • 2009
  • The volatile compounds of dried sancho (Zanthoxylum schinifolium), an aromatic plant were extracted by simultaneous distillation and extraction (SDE) method and identified by gas chromatograph-mass spectrometry (GC-MS). Selected chiral constituents of sancho oil were characterized by enantiodifferentiation using multidimensional gas chromatograph (MDGC)-MS. A total of 57 compounds were identified and quantified, and the major compounds were identified estragole, nonanoic acid, octanoic acid, $\beta$-phellandrenene, and limonene. Among them, estragol (63.9%) was found as the predominantly abundant component of sancho. $\alpha$-pinene and nerolidol, and $\beta$-pinene and linalool were determined to be enantiomerically pure (100%) for their (S)-form and (R)-form, respectively. The enantiomeric composition of limonene in sancho revealed 83.9% purity for the (S)-enantiomer, whereas (E)- and (Z)-rose oxides showed mixtures of both enantiomers. The enantiomeric excess (%) for citronellal was 22.6% with the (R)-enantiomer as major enantiomer. The enantiomeric composition of these compounds can be used as parameter for authenticity control of sancho.

Analysis of Aroma Components from Zanthoxylum

  • Chang, Kyung-Mi;Kim, Gun-Hee
    • Food Science and Biotechnology
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    • v.17 no.3
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    • pp.669-674
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    • 2008
  • Zanthoxylum schinifolium and Zanthoxylum piperitum A.P. DC. belong to the Rutaceae family and are perennial, aromatic, and medicinal herbaceous plants. In this study, their aroma compounds were isolated by steam distillation extraction using a Clevenger-type apparatus, and then further analyzed by gas chromatography (GC) and gas chromatograph/mass spectrometry (GC/MS). The yields of the essential oils from Z. schinifolium and Z. piperitum AP. DC. were 2.5 and 2.0%(w/w), respectively, and the color of their oils was quite similar, a pale yellow. From the distilled oil of Z. schinifolium, 60 volatile compounds which make up 87.24% of the total composition were tentatively identified, with monoterpenes predominating. $\beta$-Phellandrene (22.54%), citronellal (16.48%), and geranyl acetate (11.39%) were the predominantly abundant components of Z. schinifolium. In the essential oil of Z. piperitum AP. DC., 60 volatile flavor components constituted 94.78% of the total peak area were tentatively characterized. Limonene (18.04%), geranyl acetate (15.33%), and cryptone (8.52%) were the major volatile flavor compounds of Z. piperitum A.P. DC.

Analysis of Volatile Organic Compounds in Water by Modified Injection Mode for Purge & Trap-GC/MS Method (Purge & Trap-GC/MS 분석법의 주입방식 개선에 의한 물 중의 휘발성 유기물 분석)

  • Jeon, Chi Wan;Lee, Sang Hak;Eum, Chul Hun
    • Journal of the Korean Chemical Society
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    • v.39 no.8
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    • pp.635-642
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    • 1995
  • Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

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Evaluation of pesticide residue analysis of dieldrin in soil using a high resolution gas chromatograph/mass spectrometer (HR-GC/MS)

  • Hwang, Jae-Bok;Park, Tae-Seon
    • Korean Journal of Agricultural Science
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    • v.43 no.4
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    • pp.634-640
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    • 2016
  • The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

Studies on the Contents of Special Components and Estimation of Purity of Sesame Oil II (참기름의 특이 성분 함량과 순도 결정에 관한 연구(제2보))

  • 노일협;임미애
    • YAKHAK HOEJI
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    • v.27 no.2
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    • pp.169-176
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    • 1983
  • The verification of genuine sesame oil can be examined by determination of the ratio of fatty acid. Fatty acids were extracted from the saponifiable substance of sesame oils. Fatty acids were methylated with the 14% boron trifluoride methanol solution and injected into a gas chromatograph with Unisole 3000 column and finally determined the molecular weight by mass spectrometry. The fatty acids in laboratory prepared sesame oils were composed mainly of oleic acid 36.7-42.8% and linoleic acid 39.0-46.6%, including palmitic acid 7.9-9.l%, stearic acid 4.1-5.6%, linoleic acid 0.1-3.0%, arachidic acid 0.5-1.0% and eicosenoic acid 0.1-0.5%. The above results allow the estimation of genuine sesame oil, mixed with rape seed oil, soybean oil, perilla oil, etc. In 53 samples, 14 samples were estimated as genuine and it was found that erucic acid was contained in 31 samples, linoeic acid was highly contained in 14, high quantity of linolenic acid was in 7 and palmitic and oleic acid were highly involved in 3.

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Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.