• Title/Summary/Keyword: GC and GC-MS method

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Determination of N,N-Dimethylformamide in Ambient Air Using Adsorption Sampling and Thermal Desorption with GC/MS Analysis (흡착-열탈착-GC/MS를 이용한 환경대기 중 N,N-Dimethylformamide 농도 측정)

  • Seo, Young-Kyo;Hwang, Yoon-Jung;Lee, Soon-Jin;Lee, Min-Do;Han, Jin-Seok;Baek, Sung-Ok
    • Journal of Korean Society for Atmospheric Environment
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    • v.26 no.4
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    • pp.357-366
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    • 2010
  • The purpose of this study is to evaluate a method for the measurement of N,N-Dimethylformamide (DMF) and to apply the method to the ambient air samples. For the determination of DMF together with other general VOCs (e.g., benzene, toluene, and xylenes), adsorption sampling and thermal desorption with GC/MS was used in this study. The sampling and analytical approaches tested in this study showed a good repeatability and linearity with lower detection limits of less than 0.35 ppb. Field measurements were carried out at three industrial sites (Daegu-Seongseo, Siwha and Banwall industrial complexes) and one residential site in Daegu city during a period from October 2006 to November 2008. DMF was detected in 71.8% of the total samples from the Seongseo industrial complex, well known for textile industry. In contrast, DMF was detected in only 20.4% and 12.9% of all the samples from the other two sites in Banwall and Siwha industrial complexes, respectively. This implies that sources of DMF should be strongly associated with textile industry. The mean concentration of DMF also appeared to be the highest in Seongseo site (5.95 ppb), followed by a residential site in Daegu (3.28 ppb), Banwall (0.88 ppb) and Siwha (0.55 ppb). In this study, we demonstrated the environmental significance of DMF in urban ambient air. To our knowledge, the DMF measurement introduced in this paper is the first case of an official report in Korea.

Major Metabolites Involved in Skin Blackening of 'Niitaka' Pear Stored under Cold Temperature (신고 배 저온 저장 중 발생하는 과피 흑변에 관여하는 주요 대사체)

  • Lee, Eun Jin
    • Horticultural Science & Technology
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    • v.32 no.3
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    • pp.359-365
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    • 2014
  • Oriental pear (Pyrus communis L. cv 'Niitaka') was stored at $0^{\circ}C$ for 5 months and major metabolites involved in blackening of the peel were analyzed by untargeted GC-MS and targeted HPLC methods. In this study, peels of sound and skin-blackened pears were analyzed and compared. Skin-blackened fruit was clearly characterized by a distinctive pattern in changes which included a decrease of malic acid, succinic acid, and ascorbic acid, while an increase of fumaric acid, threonine, and gluconic acid, which indicated both reduced metabolic activity and anti-oxidative capacity of the cells. Chlorogenic acid was a major phenolic compound and the peel of sound fruit showed high levels of free phenolic compounds compared than the peel of skin-blackened fruit which are believed to be related to oxidation of phenolics in skin-blackened tissue. The changes or profiling of major metabolites by targeted or untargeted analysis method could become a useful tool for understanding physiology, disorder mechanism, and identifying metabolic networks connecting primary and secondary metabolism in postharvest research.

Identification of Volatile Compounds of 4 Grape Species by Storage Conditions (전자코와 GC/MS를 이용한 포도 품종별 저장 조건에 따른 휘발성 향기 성분 연구)

  • Lee, Yun-Jeung;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.7
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    • pp.874-880
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    • 2007
  • Volatile flavor compounds of 4 grape species (Campbell, Sheridan, Red globe, and Meoru) were identified during 3-day storage at either $4^{\circ}C$ or room temperature. Each sample was analyzed by solid-phase micro-extraction (SPME) method combined with gas chromatography-mass spectrometry. Also electronic nose composed of 12 different metal oxide sensors was used to differentiate flavors of grapes. Sensitivities (delta $R_{gas}/R_{air}$) of sensors from electronic nose were obtained by principal component analysis (PCA). Proportion of the first principal component was 99.30% at $4^{\circ}C$ and 99.36% at room temperature, respectively. In our result, flavor patterns of grape can be differentiated according to the storage period. The major volatile flavor compounds were 1-hexanol, hexanoic acid and its ethyl ester, and phenylethyl alcohol with the presence of butanoic acid and its ethyl ester, acetic acid, benzeneacetic acid and its ethyl ester.

Inhibitory Activity of Oak Pyroligneous Liquor against Coleosporium Plectranthi, an Obligate Parasite Responsible for the Rust Disease on Perilla Leaf

  • Kumar, Varun;Chauhan, Anil Kumar;Baek, Kwang-Hyun;Kang, Sun-Chul
    • Korean Journal of Environmental Agriculture
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    • v.30 no.4
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    • pp.453-458
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    • 2011
  • BACKGROUND: Coleosporium plectranthi, an obligate parasite, which is responsible for the rust disease of Perilla frutescens, a plant in Korea, commonly known as Perilla. All rusts are obligate parasites, meaning that they require a living host to complete their life cycle. They generally do not kill the host plant but can severely reduce growth and yield. Food and feed spoilage fungi cause great economic losses worldwide. It is estimated that between 5 and 10% of the world food production is wasted due to fungal deterioration. Rust disease of Perilla is highly frequent and is widely spread in Korea. The present study was designed to investigate a novel media for the urediniospore germination in vitro and anti-rust activity as well as GC-MS analysis of oak pyroligneous liquor. METHOD AND RESULTS: Urediniospores were collected from the infected leaf of Perilla. Spore suspension was made and the suspension was inoculated in the 2% water agar media with proper humidity, then they were incubated at $26^{\circ}C$ for 56 hrs. The GC-MS analysis of the oak pyroligneous liquor was also done to check the chemical composition. GC-MS analysis of the wood vinegar was found 15 compounds, among them o-mthoxyphenol (25.93%), 2,6-dimethoxyphenol (16.06%), 4-methylenecyclohexanone (10.69%), 2,3-dihydroxytoluene (7.84%), levoglucosane (6.14%) and propanoic acid (5.32%) were the major components. Different concentration of the oak pyroligneous liquor was used, and spore inhibition was recorded on the basis of spore counting. The best results were noted at the concentration of 50% solution where 31.8% spores were inhibited. CONCLUSION: On the basis of the chemical composition of the oak pyroligneous liquor and the activity recorded we can use it as an anti-rust agent.

Monitoring of Pesticide Residues and Risk Assessment of Agricultural Products Consumed in South Korea (국내유통농산물 중 잔류농약 모니터링 및 안전성 평가)

  • Kim, Sung-Hun;Choe, Won-Jo;Baik, Yong-Kyoo;Kim, Woo-Seong
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.37 no.11
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    • pp.1515-1522
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    • 2008
  • Monitoring the pesticide residues in agricultural products is essential to protect consumers, obtain data for risk assessment, and ensure fair trade practices. We developed a multi-residue method for the analysis of 37 pesticides with different physico-chemical properties in agricultural products and analyzed the amount of pesticide residues on about 1,000 samples circulated in South Korea. The samples consisted of 26 different types of agricultural products selected at markets in 14 major cities; cereals (2 species), nuts (1 species) potatoes (1 species), beans (2 species), fruits (3 species), vegetables (16 species), and mushrooms (1 species). In this study, residual pesticides were detected in 23 samples (2.2%) and one sample was detected to be over maximum residue limits (MRLs, 0.1%) for pesticides in foods by the Korea food code. In leafy vegetables such as pepper leaves, radish leaves, cham-na-mul, shin-sun-cho, crown daisy, chwi-na-mul and citrus fruits such as kumquat, 8 kinds of pesticides were detected. Specially, diazinon were detected over MRLs and also, endosulfan, ethoprophos and phenthoate were detected frequently. Based on these results, we investigated the risk assesment from amount of residual pesticide, total %ADI was 1.262%, but the value has not effected on human health.

Quantitative Analysis of Pentachlorophenol in Paper Products (종이재 중의 Pentachlorophenol 정량 분석)

  • Hahn, Airan;Park, Jihye;Choi, Hyeongki;Hong, Sungyeap;Han, Hyechul;Jo, Byoungmuk;Oh, Jungsoo
    • Applied Chemistry for Engineering
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    • v.16 no.3
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    • pp.323-327
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    • 2005
  • Pentachlorophenol (PCP) is a representative compound of chlorophenol derivatives which are especially toxic and potentially carcinogenic compounds in the priority pollutant list of the EPA (Environmental Protection Agency, USA). The aim of this study was to investigate an analysis method of PCP in infinitesimal quantity retained in paper. PCP in paper was pretreated by solid phase extraction (SPE) in a phenyl cartridge. The extracted sample was acetylated or silylated and analyzed with GC/MS-SIM. The detection sensitivity of silylated PCP was improved significantly when compared with those of PCP itself and acetylated PCP. As a test specimen, an office paper and a wallpaper were used.

GC/MS Analysis of Ethylene Glycol in the Contaminated Lubricant Oil Through Solvent Extraction Followed by Derivatization using Bistrimethylsilyltrifluoroacetamide (BSTFA) (엔진윤활유 중 Ethylene Glycol의 용제추출후 bistrimethylsilyltrifluoroacetamide(BSTFA)를 이용한 GC/MS 분석에 관한 연구)

  • Lee, Joon-Bae;Kwon, O-Seong;You, Jae-Hoon;Shon, Shungkun;Sung, Tae-Myung;Paeng, Ki-Jung
    • Tribology and Lubricants
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    • v.28 no.6
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    • pp.315-320
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    • 2012
  • For proper functioning, general machines usually need lubricant oil as a cooling, cleaning, and sealing agent at points of mechanical contact. The quality of lubricant oil can deteriorate during operation owing to various causes such as high temperature, combustion products and extraneous impurities. In this study, a heavy load stopped during operation, and the oil was analyzed to check whether any impurities were added. Extraction using acetonitrile followed by reaction with BSTFA(bistrimethylsilyl trifluoroacetamide) showed that, trimethylsilylated ethylene glycol was present in the lubricant oil. To quantify the ethylene glycol in the oil, deuterium-substituted ethylene glycol, which acted as an internal standard, was added to the sample and then extracted with the solvent. Next, the extract was reacted with the derivatizing agent(BSTFA) and then analyzed with GC/MS. The detection limit of this method was found to be $0.5{\mu}g/g$ and the recovery of oil containing $20,000{\mu}g/g$ of ethylene glycol was measured to be 94.8%. A damaged O-ring and eroded cylinder liner were found during the overhaul, which implied the leakage of coolant containing ethylene glycol into the lubricating system. The erosion of the cylinder liner was assumed to be due to cavitation of the coolant in the cooling system.

Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법)

  • Hong, Jongki;Baek, In-Girl;Kim, Hyub;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Park, Hyun-Mee;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.666-674
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    • 2000
  • The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

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Uncertainty Evaluation of the Analysis of 11-Nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol in Human Urine by GC/MS (GC/MS를 이용한 소변 중 대마 대사체 분석의 측정불확도 평가)

  • Kim, Jin-Young;Jeong, Jae-Chul;Suh, Sung-Ill;Suh, Yong-Jun;Lee, Jeong-Jik;Kim, Jong-Sang;In, Moon-Kyo
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.480-487
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    • 2008
  • We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH), the major metabolite of ${\Delta}^9$-tetrahydrocannabinol, in urine sample by solid-phase extraction (SPE) and GC/MS detection. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day and inter-person validation were performed using statistical analysis of several indicative factors. Measurement uncertainty associated with target analyte in real forensic samples was estimated using quality control (QC) data. Traceability of measurement was established through traceable standards, calibrated volumetric glassware and volume measuring device. The major factors of contribution to combined standard uncertainty, were calibration linearity, inter-day repeatability and inter-person reproducibility, while those associated with preparation of analytical standards and sampling volume were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method was 12.05% for THCCOOH.

Determination of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Capillary-GC(FID) (Capillary-GC(FID)에 의한 오미자 Lignan 성분의 정량)

  • Sohn, Hyun-Joo;Bock, Jin-Young;Baik, Soon-Ok;Kim, Yong-Ha
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.350-356
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    • 1989
  • The determinabilities of several lignan compounds by capillary-GC (F1D) were studied. The lignan compounds used were deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H and tigloylgomisin H which were isolated from fruits of Schisandra chinensis BAILLON and identified with GC/MS(EI, 70eV), 1H-NMR(300MHz) and IR. The GC column used was SPB-1 fused silica capillary$(0.25mm\;ID{\times}30m,\;Supelco)$, and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute. The linearities between concentration and FID response were maintained in $2{\sim}500ppm$ of deoxyschizandrin and wuweizisu C and in $5{\sim}500ppm$ of gomisin N, schizandrin, gomisin A, angeloylgomisin H and tigloylgomisin H. The contents of lignan compounds in fruits of S. chinensis BAILLON produced at Moo-ju area were analyzed by the GC method: the values obtained of schizandrin and gomisin N were 6.5 and 5.9mg/g respectively, and those of gomisin A, wuweizisu C, angeloylgomisin H, deoxyschizandrin and tigloylgomisin H were $0.5{\sim}1.6mg/g$.

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