• Title/Summary/Keyword: HS-SPME

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Volatile Metabolic Markers for Monitoring Pectobacterium carotovorum subsp. carotovorum Using Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

  • Yang, Ji-Su;Lee, Hae-Won;Song, Hyeyeon;Ha, Ji-Hyoung
    • Journal of Microbiology and Biotechnology
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    • v.31 no.1
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    • pp.70-78
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    • 2021
  • Identifying the extracellular metabolites of microorganisms in fresh vegetables is industrially useful for assessing the quality of processed foods. Pectobacterium carotovorum subsp. carotovorum (PCC) is a plant pathogenic bacterium that causes soft rot disease in cabbages. This microbial species in plant tissues can emit specific volatile molecules with odors that are characteristic of the host cell tissues and PCC species. In this study, we used headspace solid-phase microextraction followed by gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS) to identify volatile compounds (VCs) in PCC-inoculated cabbage at different storage temperatures. HS-SPME-GC-MS allowed for recognition of extracellular metabolites in PCC-infected cabbages by identifying specific volatile metabolic markers. We identified 4-ethyl-5-methylthiazole and 3-butenyl isothiocyanate as markers of fresh cabbages, whereas 2,3-butanediol and ethyl acetate were identified as markers of soft rot in PCC-infected cabbages. These analytical results demonstrate a suitable approach for establishing non-destructive plant pathogen-diagnosis techniques as alternatives to standard methods, within the framework of developing rapid and efficient analytical techniques for monitoring plant-borne bacterial pathogens. Moreover, our techniques could have promising applications in managing the freshness and quality control of cabbages.

Composition and Cell Cytotoxicity of Essential Oil from Caryopteris incana Miq. in Korea (층꽃나무(Caryopteris incana Miq) 정유의 성분 분석과 세포 독성 평가)

  • Kim, Song-Mun
    • Applied Biological Chemistry
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    • v.51 no.3
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    • pp.238-244
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    • 2008
  • The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

Determination of the presence of benzene in vitamin drinks using headspace - solid phase microextraction and gas chromatography - mass spectrometry (Headspace Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry를 이용한 비타민드링크 제품 중 Benzene의 미량분석)

  • Kim, Jong-Hun;Lee, Kyung-Min
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.237-245
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    • 2007
  • The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

Relationship between NVOCs Concentration and Korean Red Pine (Pinus densiflora S. et Z.) Forest Environment in Spring Season (봄철 소나무숲의 NVOC 농도와 숲환경과의 상관관계)

  • Kim, GeonWoo;Kwon, ChiWon;Yeom, DongGeol;Joung, Dawou;Choi, Yoon Ho;Park, Bum-Jin
    • Journal of Korean Society of Forest Science
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    • v.103 no.3
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    • pp.483-489
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    • 2014
  • This study aimed at a scientific examination of the relationship between NVOCs concentration and the physical environment of red pine forest in spring season. Atmospheric NVOC samples in red pine forest was collected through five trials conducted from March to May 2013, using Tanax-Ta-charged disposable tubes and mini-pumps. At each trial, measurements were taken at three different points in daytime (sunrise, southing and sunset). For maximum accuracy, two tubes were used for each measurement at the same location, and the mean value was used for analysis. Compound analysis on the NVOC samples was done using the HS-SPME method and GC-MS. Analysis of the relationship between NVOC and the physical forest environment found higher concentrations of most substances, including ${\alpha}$-pinene and ${\beta}$-pinene, with higher temperature, dew point, and lower concentrations with higher wind velocity. The findings of this study offer scientific evidence which can inform the creation of 'healing forests' and 'recreational forests' as well as forest environment in general, helping to promote public health and recreational activities.

Effects of Treatments on the Distribution of Volatiles in Artemisia princeps Pampan (쑥의 처리조건에 따른 휘발성 성분 변화)

  • Park, Min-Hee;Kim, Mi-Ja;Cho, Wan-Il;Chang, Pahn-Shick;Lee, Jae-Hwan
    • Korean Journal of Food Science and Technology
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    • v.41 no.5
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    • pp.587-591
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    • 2009
  • Volatiles in Artemisia princeps Pampan. cv. sajabal (sajabalssuk) and A. princeps Pampan. (ssuk) treated with different processing were analyzed using headspace-solid phase microextraction (HS-SPME)/gas chromatography- a mass selective detector (GC-MS). Sajabalssuk and ssuk were treated with steam distillation (SD) and freeze-dried/steam distillation (FD/SD) while controls were raw sajabalssuk and raw ssuk. Sajabalssuk had significantly more total volatiles than ssuk in control and FD/SD treated samples (p<0.05). Major volatiles in raw sajabalssuk were 2-hexenal, 1,8-cineol, trans-caryophyllene, and hexanal while those in raw ssuk were 1-hexanol, ${\beta}$-myrcene, limonene, and 2-hexenal, which implies that substantial lipid oxidation occurred in raw samples. Sajabalssuk with SD and FD/SD treatment had higher peak areas of 1,8-cineole, 4-terpineol, 1-octen-3-ol, and ${\alpha}$-terpineol while ssuk with SD and FD/SD treatment possessed 1,8-cineol, camphor, borneol, artemisia ketone, ${\alpha}$-thujone, and 1-octen-3-ol, which showed that steam distillation produced more volatiles from terpenoids than raw samples. Based on the results of HS-SPME/GC-MS, relative amounts of volatiles from lipid oxidation including 2-hexenal, hexanal, and 1-hexanol were reduced in sajabalssuk and ssuk with freeze-drying and/or steam distillation treatment.

Simultaneous determination of 37 volatile organic compounds at ng/L concentration level in surface water by HS-SPME-GC/MS (HS-SPME-GC/MS에 의한 지표수에서 ng/L 농도 수준의 37개 휘발성유기화합물의 동시 분석)

  • Kim, Tae-Seung;Hong, Suk-Young;Kim, Jong-Eun;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.39-49
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    • 2012
  • A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

Volatile organic components of gel pen inks by HS-SPME GC/MS (HS-SPME GC/MS를 이용한 젤펜잉크의 휘발성 성분)

  • Kim, Chang-Seong;Choi, Mi-Jung;Sun, Yale-Shik;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.423-428
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    • 2010
  • In this study, VOCs of black gel pen inks was screening to identify individual characteristic of gel pen inks. Detected VOCs was total 20 species(isopropylalcohol, 2-methyl-2-propanol, 2-butanone, hydrazinecarbothioamide, benzeneacetic acid (ethyl ester), benzeneacetic acid, dimethoxymethy-silane, 2,2-dimethoxybutane, tetrahydro-2-methyl-furan, 1,2-ethanediol, silicic acid (tetramethyl ester), 1,2-propanediol, propyleneglycol, 3-ethyl-3-hexanol, 1,1-dipropoxy-propane, 2-butoxy-ethanol, 2,2'-oxybisethanol, 1-butyl-benzene, 2-pyrrolidinone, 2-(2-butoxyethoxy)-ethanol). We detected 2,2-dimethoxybutane (3.02~47% ratio) and tetrahydro-2-methyl-furan (1.19~52.19% ratio), 1,2-ethanediol (52.83~95.84% ratio). In case of manufacturer, manufactured ink was able to discriminate between Japan and Korea by distinct characteristics (Japan: 1,2-ethanediol, 52.83~95.84%, Korea: 1,2-propanediol, 76.17~93.51%). The results of this study indicated that distinct characteristic about manufacturers and brands could make a classifring tool of inks for identification of between gel pen inks.

Impacts of Coffee Creamer, Dried Skim Milk and Sugar on the Volatile Aroma Compounds and Sensory Characteristics in Instant Coffee (인스턴트커피에 커피크리머, 탈지분유, 설탕의 첨가가 휘발성향기성분과 맛에 미치는 영향)

  • Min, Ji-Sook;Kwon, Hye-Min;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.47 no.2
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    • pp.137-144
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    • 2015
  • Although instant coffee is less palatable than freshly brewed coffee, it is widely consumed primarily due to its convenience. Frequently, instant coffee is consumed in the form of a coffee-mix. It contains coffee creamer or dried skim milk, and sugar in addition to soluble coffee. The aim of this study was to investigate the volatile aroma compounds (VACs) of instant black coffee mixed with coffee creamer or dried skim milk by Gas Chromatography-Headspace-Solid Phase Microextraction (GC-HS-SPME) and sensory evaluation. A total of 16 different coffee samples including instant black coffee and coffee mixes with coffee creamer or dried skim milk, were chosen for this study. The coffee samples contained several common VACs such as pyrazine, pyridine, and pyrrole. Sensory evaluation indicated that the flavor intensity of coffee mix was less pronounced than that of instant black coffee alone. Coffee creamer and skim milk had little distinctive aroma per se; however, they significantly contributed to the flavor profile of coffee mixes, suggesting that coffee creamer and skim milk acted as flavor modifiers in coffee mix.

Studies on the Free and Bound Aroma Compounds in Green and Fermented Teas (녹차와 후발효차의 유리형 및 결합형 향기성분에 대한 연구)

  • Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.43 no.4
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    • pp.407-412
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    • 2011
  • Free and bound aroma compounds in green and fermented teas treated with microbial-fermentation were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. Aldehydes and ketones in green tea decreased during microbial fermentation, whereas linalool and geraniol increased in the fermented tea. After enzyme treatment, (Z)-3-hexen-1-ol increased significantly following enzymatic hydrolysis of both green and fermented teas. In addition, benzaldehyde, 3-hexenyl acetate, and geraniol also increased in green tea with enzyme treatment. Bound aroma compounds in the green and fermented teas increased at different levels of added enzyme. We demonstrated the enhancement of both green and fermented teas by enzyme treatment, which can lead to improvement in the flavor qualities of green and fermented teas.

Profiling Patterns of Volatile Organic Compounds in Intact, Senescent, and Litter Red Pine (Pinus densiflora Sieb. et Zucc.) Needles in Winter

  • CHOI, Won-Sil;YANG, Seung-Ok;LEE, Ji-Hyun;CHOI, Eun-Ji;KIM, Yun-Hee;YANG, Jiyoon;PARK, Mi-Jin
    • Journal of the Korean Wood Science and Technology
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    • v.48 no.5
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    • pp.591-607
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    • 2020
  • This study was aimed to investigate the changes of chemical composition of the volatile organic compounds (VOCs) emitted from red pine needles in the process of needle abscission or senescence. The VOCs in intact, senescent, and litter red pine needle samples were analyzed by headspace-solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC/MS). And then, multivariate statistical interpretation of the processed data sets was conducted to investigate similarities and dissimilarities of the needle samples. Principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA) were used to investigate the dataset structure and discrimination between samples, respectively. From the data preview, the levels of major components of VOCs from needles were not significantly different between needle samples. By PCA investigation, the data reduction according to classification based on the chlorophyll a / chlorophyll b (Ca/Cb) ratio were found to be ideal for differentiating intact, senescent, and litter needles. The following OPLS-DA taking Ca/Cb ratio as y-variables showed that needle samples were well grouped on score plot and had the significant discriminant compounds, respectively. Several compounds had significantly correlated with Ca/Cb ratio in a bivariate correlation analysis. Notably, the litter needles had a higher content of oxidized compounds than the intact needles. In summary, we found that chemical compositions of VOCs between intact, senescent, and litter needles are different each other and several compounds reflect characteristic of needle.