• Title/Summary/Keyword: Solid-phase microextraction

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Studies on the anodic oxidation of some volatile organic halogen compounds(THM) (휘발성 할로겐 화합물(THM)의 양극 산화에 관한 연구)

  • Yoo, K.S.;Park, S.Y.;Yang, S.B.;Woo, S.B.
    • Analytical Science and Technology
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    • v.10 no.4
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    • pp.264-273
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    • 1997
  • Anodic oxidation reaction was applied to remove trihalomethanes in an aqueous solution. Each component was determined by using solid phase microextraction(SPME) fiber and GC-ECD. Anodic and cathodic compartments were separated in order to protect contaminants and connected by $KNO_3$-agar bridge. The calibration graphs of the 6 THM components were shown good linearlity from a few ppb up to a few hundreds ppb concentration level. Anodes such as platinum(Pt), titanium(Ti). zircornium(Zr), titanium metal coated with iridium(Ti-Ir), and glassy carbon coated with mixed valence ruthenium(mv Ru) were tried to remove the THMs at different potentials. The best result was obtained on the Ti-Ir anode applied 9 volts DC. The electrode could effectively remove almost all the THM components from the stirring solution within about 1.5 hours. The glassy carbon electrode coated with mixed valence ruthenium showed excellent removing effect at the begining, but the maximum removing level was remained at 60% probably due to the destruction of the electrode surface. The concentration of chloroform, however, tends to be increased due to the electrode reaction producing the component at the condition.

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Frangrance and Chemical Composition of Essential Oil in Cone of Metasequoia (Metasequoia glyptostroboides Hu et Cheng) (메타세콰이아 (Metasequoia glyptostroboides)구과(毬果) 정유의 향취 및 휘발성 화학성분)

  • Yeon, Bo-Ram;Cho, Hae-Me;Jeong, Mi-Soon;Kim, Song-Mun
    • Korean Journal of Weed Science
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    • v.31 no.2
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    • pp.146-151
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    • 2011
  • Essential oil was extracted from cones of metasequoia (Metasequoia glyptostroboides) by steam distillation, fragrance was determined by sensorial analysis and chemical compositions were analyzed by gas chromatography-mass spectrometry with solid-phase microextraction apparatus. Metasequia contained 0.40% of essential oil in the cone. Major impact fragrances of the essential oil were woody, coniferous and herbal, and minor impact fragrances were minty, spicy and oily. There were nine constituents in the essential oil : 8 hydrocarbons and 1 oxide. Constituents were limonene (66.18%), ${\delta}$-3-carene (11.11%), ${\beta}$-caryophyllene (6.66%), ${\beta}$-myrcene (5.92%), ${\beta}$-pinene (4.14%), caryophyllene oxide (2.39%), camphene (2.32%), ${\alpha}$-caryophyllene (0.85%), and tricyclene (0.43%). Herbal and minty frangrances could be due to limonene and ${\delta}$-3-carene, spicy frangrance to caryophyllene, woody and coniferous frangrances to ${\alpha}$-pinene and ${\beta}$-pinene, and oily fragrance to camphene.

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.

Determination of benzene, toluene, ethylbenzene and o-xylene in bottled waters by headspace solid-phase microextraction and gas chromatography/mass spectrometry (HS-SPME-GC/MS를 이용한 먹는 샘물 중 벤젠, 톨루엔, 에칠벤젠, 자일렌의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.119-126
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    • 2011
  • Abstract: The amount of benzene, toluene, ethylbenzene, and o-xylene (BTEX) in 30 kinds of bottled waters purchased from market and 9 kinds of tap waters from home were determined using headspace solid phase microextraction (HS-SPME). The sample was stirred at 1200 RPM G for 4 min using a magnetic bar with $100\;{\mu}m$ PDMS as adsorbent for BTEX. Then it was desorbed from the fiber for 1 min at room temperature. Quantitation was achieved using standard calibration method. The limit of detection was determined as benzene 0.39 (${\pm}0.04$) ng/mL, toluene 0.08 (${\pm}0.04$) ng/mL, ethylbenzene 0.04 (${\pm}0.01$) ng/mL, and o-xylene 0.05 (${\pm}0.02$) ng/mL. Benzene and o-xylene were not detected in any samples, but toluene was detected in 11 samples, and ethylbenzene was detected just in 3 samples among 30 investigated bottled waters. The concentration range of investigated materials for toluene and o-xylene were $0.24({\pm}0.09)\sim2.95\;({\pm}0.08)\;ng/mL$, $0.08({\pm}0.06)\sim0.93({\pm}0.10)\;ng/mL$, respectively.

Volatile Changes in Beverages and Encapsulated Powders Containing an Artemisia Extract during Production and Storage (쑥 추출물 함유 음료와 미세캡슐의 제조 및 저장 중 휘발성분 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.43 no.3
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    • pp.271-276
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    • 2011
  • Volatile profiles of beverages and encapsulated powders containing Artemisia princeps Pampan extracts were analyzed by solid-phase microextraction-gas chromatography/mass spectrometry during production and storage. Beverages containing 0.32 and 0.64% extracts were stored at room temperature for 8 weeks and $60^{\circ}C$ for 8 days, respectively. Encapsulated particles were stored at room temperature and $60^{\circ}C$ for 8 days. Total volatiles in beverages decreased significantly during storage, irrespective of storage condition (p<0.05). Terpenoids, including cymene, thujone, and ${\beta}$-myrcene, were major volatiles in beverages, and some volatiles including ethylfuran, vinylfuran, and 2-fufural increased in 60oC samples only. Total volatiles in microcapsules at room temperature were not significant different for 8 days (p>0.05), whereas those at $60^{\circ}C$ increased by 16.5 times. Limonene was the most detected volatile in microcapsules, and aldehydes such as hexanal, pentanal, and octanal, and furans such as 2-butylfuran and 2-pentylfuran increased in the $60^{\circ}C$ samples, which may have originated from oxidized lipids used in the microcapsules.

Flavor Components of Mideoduck (Styela clava) (미더덕의 향기 성분)

  • Choi, Byeong-Dae;Oh, Bong-Se;Kang, Seok-Joong
    • Journal of Life Science
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    • v.20 no.11
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    • pp.1648-1655
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    • 2010
  • The flavor extracts of Mideoduck muscle and its juices were concentrated by simultaneous distillation and extraction (SDE) and solid-phase microextraction (SPME) methods. Each component present in the extracts was identified with GC and GC-MS by the n-paraffin hydrocarbon retention index and standard MS library data system. By SDE, $371.3\;{\mu}g/g$ of hexanal, $80.1\;{\mu}g/g$ of 1-tridecanol, $72.1\;{\mu}g/g$ of (Z)-4,5-dimethylhex-2-en-4-ol with other alcohols, aldehydes and acids were present in the flavor extracts, with the alcohols having the highest composition and being the most important factor in Mideoduck muscle flavor. By SPME, 9 alcohols, 1 acid, 1 aldehyde, 1 hydrocarbon, 1 ester, 1 amine and 2 ketones were detected in the extracts, with alcohol such as 1-nonanol, 1-decanol and 1-tridecanol as the major components. In SPME, the muscle sample, consisting of $31.6\;{\mu}g/g$ of 1-nonanol, $20.3\;{\mu}g/g$ of (E)-2-butenedioic acid dibutylester, and $26.7\;{\mu}g/g$ of heptadecanoic acid made up the 62.1% of total flavor extracts of Mideoduck muscle. The results of the SPME methods were similar to the composition of the raw material flavor of the sample even at a low concentration.

Volatile Compounds in the Oxidation of Unsaturated Fatty Acids Caused in Off-flavor of Porcine Liver by HS-SPME (Headspace solid-phase microextraction(HS-SPME)를 이용한 간의 비린내불쾌취에 기인하는 불포화지방산 산화생성물의 휘발성성분)

  • Im, Sung-Im;Choi, Sung-Hee
    • Korean Journal of Food Science and Technology
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    • v.35 no.3
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    • pp.359-365
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    • 2003
  • Headspace solid-phase microextraction(HS-SPME) was used to isolate the off-flavor volatile compounds, which are formed during the oxidation of porcine liver and unsaturated fatty acids in porcine liver induced by iron. Three fibers for HS-SPME method development were tested, and the polydimethylsiloxane/divinylbenzene(PDMS/DVB) fiber was selected as providing the best detection of analyzed compounds. In the oxidized arachidonic acid, the major compounds identified were hexanal, 1-octen-3-one(metallic), (Z)-4-heptenal, (E)-2-octenal, 1-octen-3-ol(mushroom), (Z)-2-nonenal (cardboard-like), and (E,E)-2,4-decadienal(fatty, oily). In the oxidized linolenic acid, the major ones were (E,E)-2,4-heptadienal(fishy), (E,E)-3,5-octadien-2-one and (E,Z)-2,6-nonadienal. Moreover, those of th oxidized porcine liver with iron were hexanal, 1-octen-3-one, (Z)-4-heptenal, (E,Z)-2,4-decadienal and (E,E)-2,4-decadienal. These results showed that the fishy and metallic off-flavor in porcine liver were due to the oxidation of unsaturated fatty acids in porcine liver.

Optimum Extraction Methods of Volatile Compounds in Beef Extract Powder (쇠고기 엑기스 분말 휘발성 성분의 최적 추출방법에 관한 연구)

  • Kim Hun;Cho Woo-Jin;Jeong Eun-Jeong;Ahn Jun-Suck;Lim Chi-Won;Yoo Young-Jae;Kim Kwang-Ho;Cha Yong-Jun
    • The Korean Journal of Food And Nutrition
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    • v.17 no.4
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    • pp.412-419
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    • 2004
  • In odor to select optimum extraction methods of volatile compounds in beef extract powder(BEP) as basic data for the development of a new detection method of irradiated BEP, four extraction methods, such as solid phase microextraction with polar fiber(S-PD) and non-polar fiber(S-CD), purge and trap(P&T) and liquid liquid continuous extraction(LLCE) methods, were tested with gas chromatography/mass spectrometry method. A total of 106 volatile compounds including 22 hydrocarbons, 7 aldehydes, 6 ketones, 13 alcohols, 6 sulfur-containing compounds, 19 nitrogen-containing compounds, 6 aromatic compounds, 17 terpenes, 8 furans and 2 miscellaneous compounds were detected in BEP by four detection methods. The most compounds(62 compounds) were detected by S-PD method, followed by P&T(43), LLCE(38) and S-CD method(30). Among these methods, S-PD and P&T methods showed a complementary interrelationship to detect volatile compounds as S-PD method showed high detectabiltiy to all compound groups except hydrocarbons and ketones, which had high volatility and low molecular weight(less than RI 1200), but P&T method showed the contrary pattern to that of S-PD method. Moreover, the most of volatile compounds detected by S-CD and LLCE methods were also detectable by S-PD or/and P&T methods. Therefore, the simultaneous application of S-PD and P&T methods were selected as the optimum volatile extraction methods of BEP.

Characteristics of Volatile Compound Adsorption from Alcoholic Model Solution onto Various Activated Carbons (알코올모델용액을 이용한 여러 종류 활성탄의 휘발성화합물 흡착특성)

  • Park, Seung-Kook;Lee, Myung-Soo;Kim, Byung-Ho;Kim, Dae-Ok
    • Food Engineering Progress
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    • v.14 no.3
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    • pp.249-255
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    • 2010
  • Ten commercial activated carbons (ACs) prepared from four different sources (bamboo, wood, peat, and coal) were evaluated for their adsorptive efficiency of six volatile compounds (isoamyl alcohol, hexanal, furfural, ethyl lactate, ethyl octanoate, 2-phenyl ethanol) which were dissolved in a 30% alcoholic model solution. These six volatile compounds are frequently found in alcoholic beverages and possibly contribute to physiological hangover due to their high concentrations. They are also generally regarded as off-flavor compounds at certain levels in alcoholic beverages such as whisky and vodka. Two hundred mL of 30% alcoholic solutions containing these six volatile compounds were treated with 0.2 g of ACs while stirring for 16 hr; the treated solutions were then measured for their adsorptive efficiencies (or removal efficiencies) by gas chromatographic analysis using two different sampling methods (direct liquid injection and headspace-solid phase microextraction). The adsorptive efficiencies of the ACs varied depending on the identity of the volatile compounds and the source material used for making the ACs. Ethyl octanoate, 2-phenyl ethanol, and hexanal were removed at high efficiencies (34-100%), whereas isoamyl alcohol, ethyl lactate, and furfural were removed at low efficiencies (5-13%). AC prepared from bamboo showed a high removal efficiency for isoamyl alcohol, aldehydes (hexanal and furfural), and 2-phenyl ethanol; these major fusel oils have been implicated as congeners responsible for alcohol hangover.

Evaluation of TVOC contribution from Raw materials of PVC wallpaper using the Headspace-SPME-GC/MS (HS-SPME-GC/MS 법을 이용한 PVC벽지 원자재의 TVOC 기여도 평가)

  • Jang, Mi-Ok;Jeong, Tak-Kyo;Jeong, Yung-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.488-495
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    • 2007
  • A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.