• Title/Summary/Keyword: headspace(HS)

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Measurement of Aldehydes in Replacement Liquids of Electronic Cigarettes by Headspace Gas Chromatography-mass Spectrometry

  • Lim, Hyun-Hee;Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2691-2696
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    • 2013
  • The electronic cigarette (E-cigarette) is a battery-powered device that aerosolizes nicotine so that it is readily delivered into the respiratory tract. The analytical data regarding the substances present in E-cigarettes are very limited. The aim of this study was to measure the concentration of aldehydes-formaldehyde (FA), acetaldehyde (AA) and, acrolein (AL)-in 225 replacement liquid brands from 17 E-cigarette shops sold in the Republic of Korea by headspace solid-phase micro extraction and gas chromatography-mass spectrometry (HS-SPME GC-MS). The concentration range of FA and AA was 0.02-10.09 mg/L (mean = 2.16 mg/L, detected in 207 of 225 samples) and 0.10-15.63 mg/L (mean = 4.98 mg/L, detected in all samples), respectively. AL was not detected in any of 225 replacement liquids. FA and AA were originally present in almost all replacement liquids of electronic cigarettes.

Essential Oil Analysis of Illicium anistum L. Extracts

  • Min, Hee-Jeong;Kim, Chan-Soo;Hyun, Hwa-Ja;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.6
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    • pp.682-688
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    • 2017
  • Fresh japanese anise (Illicium anisatum L.) tree leaves were collected and ground after drying. The essential oils of the leaves were analyzed by gas chromatography-mass spectrometry (GC-MS) using headspace (HS) and solid phase-microextra (SPME) methods. Volatile components of the leaves were identified 21 and 65 components in HS and SPME, respectively. The main components of the essential oils obtained by HS method were eucalyptol (36.7%), (+)-sabinene (15.61%), ${\delta}$-3-carene (6.87%), ${\alpha}$-pinene (6.07%), ${\gamma}$-terpinen (5.72%), ${\alpha}$-limonene (5.26%), ${\beta}$-myrcene (4.13%), ${\alpha}$-terpinene (4.04%) and ${\beta}$-pinene (3.73%). The other components were less than 3.5%. SPME method also showed that eucalyptol (17.88%) was main. The other were 5-allyl-1-methoxy-2 (13.29%), caryophyllene (6.09%), (+)-sabinene (5.60%), ${\alpha}$-ocimene (4.89%) and ${\beta}$-myrcene (3.73%), and the rest were less amounts than 3.5%. This work indicated that many more volatile components were isolated, comparing to the previous literature data and that SPME method was much more effective than HS method in the analysis of the volatile components.

Mulberry Paper Bag μ-Solid Phase Extraction for the Analysis of Five Spice Flavors by Gas Chromatography-Mass Spectrometry

  • Yoon, Ok-Kyung;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.35-42
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    • 2009
  • Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

Determination of Volatile Organic Compounds in Waste using HS/GC/MS Analysis (Headspace/GC/MS를 이용한 폐기물중 휘발성 유기화합물의 분석)

  • Kim, Kyeo-Keun;Shin, Sun-Kyoung;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.72-80
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    • 2000
  • The HS/GC/MS method was performed to analyze the volatile organic compounds in waste sludge samples. This study was performed to establish the fundamental data by studying the effects of salt, equilibrium temperature and time in the volatile organic compounds analysis. The presence of salts have been found to increase the sensitivity. The peak area is increased from 1.07 to 2.61 times by adding the salts to the water sample, compared with a salt tree sample. The recoveries of target compounds have found between 90% and 127% at sample temperature of $85^{\circ}C$ for 30 min. This HS/GC/MS method can be applied to analyze the volatile organic compounds and organohalo compounds in the environmental matrix.

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Analysis of Haloacetonitriles in Drinking Water Using Headspace-SPME Technique with GC-MS (Handspace Solid Phase Microextraction 방법에 의한 HANs 분석에 관한 연구)

  • Cho, Deok-Hee
    • Journal of Korean Society of Water and Wastewater
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    • v.18 no.5
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    • pp.628-637
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    • 2004
  • In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of disinfection by-products (DBPs) such as haloacetonitriles (HANs), trihalomethanes (THMs), haloacetic acids (HAAs). In this study, headspace-solid phase microextraction (HS- SPME) technique was applied for the analysis of HANs in drinking water. The effects of experimental parameters such as selection of SPME fiber, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and detection limits were also evaluated. The $50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were the optimal experimental conditions for the analysis of HANs. The correlation coefficients ($r^2$) for HANs was 0.9979~0.9991, respectively. The relative standard deviations (%RSD) for HANs was 2.3~7.6%, respectively. Detection limits (LDs) for HANs was $0.01{\sim}0.5{\mu}g/L$, respectively.

Determination of volatile compounds by headspace-solid phase microextraction - gas chromatography / mass spectrometry: Quality evaluation of Fuji apple

  • Lee, Yun-Yeol;Jeong, Moon-Cheol;Jang, Hae Won
    • Analytical Science and Technology
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    • v.30 no.2
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    • pp.68-74
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    • 2017
  • The volatile components in 'Fuji' apple were effectively determined by a headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 48 volatile components were identified and tentatively characterized based on National Institute of Standards and Technology (NIST) MS spectra library and the Kovats GC retention index I (RI). The harvested Fuji apples were divided into two groups: 1-methylcyclopropene (1-MCP) treated and non-treated (control) samples for finding important indicators between two groups. The major volatile components of both apples were 2-methylbutyl acetate, hexyl acetate, butyl 2-methylbutanoate, hexyl butanoate, hexyl 2-methylbutanoate, hexyl hexanoate and farnesene. No significant differences of these major compounds between 1-MCP treated and non-treated apples were observed during 1 month storage. Interestingly, the amount of off-flavors, including 1-butanol and butyl butanoate, in 1-MCP treated apples decreased over 5 months, and then increased after 7 months. However, non-treated apples did not show significant changes for off-flavors during 7 month storage (p<0.05). The non-treated apples also contained the higher levels of two off-flavors than 1-MCP treated apples. These two compounds, 1-butanol and butyl butanoate, can be used as quality indicators for the quality evaluation of Fuji apple.

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.

Effects of Broth pH and Chilling Storage on the Changes in Volatile Profiles of Boiled Chicken Flesh

  • Pattarabhorn Pakaweerachat;Teerin Chysirichote
    • Food Science of Animal Resources
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    • v.44 no.5
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    • pp.1096-1107
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    • 2024
  • This study investigated the changes in volatile compounds in chicken flesh after boiling at various pHs (6.0-9.0) and after chilling storage (4.0±1.0℃) for 7 d. The volatile compounds were assessed qualitatively and quantitatively by using a headspace gas chromatography-mass spectrometry analysis. Twenty-one volatile compounds were discovered and categorized as amine, aldehyde, alcohol, ketone, acid, and furan. One type of amine, (2-aziridinylethyl) amine, was the most prevalent volatile component, followed by aldehyde, ketone, aldehyde, acid, ester, and furan. The results showed that the quantity and quality of the volatile compounds were influenced by a pH of the boiling medium. Additionally, the types and volatile profiles of the chicken were altered during chilling. In particular, in the chicken that was boiled at a pH of 8.0, the hexanal (an aldehyde) content increased the most after 7 d of chilling. Moreover, various alcohols formed after the 7 d of chilling of the chicken that was boiled at pHs of 8.0 and 9.0. Because of the oxidation and degradation of fat and proteins, the most altering volatile compounds were the reducing amines and the increasing aldehydes.

Determination of geosmin and 2-MIB in Nakdong River using headspace solid phase microextraction and GC-MS (HS-SPME-GC/MS를 이용한 낙동강 수계 하천수 중 조류기원성 냄새물질 분석)

  • Lee, Injung;Lee, Kyoung-Lak;Lim, Tae-Hyo;Park, Jeong-Ja;Cheon, Seuk
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.326-332
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    • 2013
  • Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

Poly(dimethylsiloxane) Mini-disk Extraction

  • Cha, Eun-Ju;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3603-3609
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    • 2011
  • A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.