• Title/Summary/Keyword: SPME-GC-O

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Changes in Volatile Compounds of Green Tea during Growing Season at Different Culture Areas (녹차엽의 채취 시기와 재배지역에 따른 휘발성 향기 성분의 변화)

  • Lee, Joo-Yeon;Wang, Li-Fei;Baik, Joo-Hyun;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.39 no.3
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    • pp.246-254
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    • 2007
  • Fresh tea leaves grown in Jeju Island and Jeonnam Province of South Korea were plucked and processed. Volatile compounds (VCs) were analyzed and identified with SPME-GC/GC-MS/GC-O. The VCs of green teas were classified into two major categories based on their aroma characteristics: the Greenish (Group I), and Floral (Group II) odorants. It was found that the VCs were decreased significantly in fresh tea leaves as they were plucked at the later stages of cultivation. The ratio of VCs responsible for Group I and Group II compounds was well-balanced in tea leaves plucked in May, but the balances were changed when the fresh leaves were processed. The major VCs of fresh tea leaves in Jeju and Jeonnam were n-hexanal, E-2-hexenal, Z-3-hexenal, myrcene, benzyl alcohol, linalool, and phenyl alcohol. Also, Jeju and Jeonnam tea leaves had different aroma composition. n-Heptanol, ${\beta}-pinene$, benzaldehyde, and ethyl salicylate were found in Jeju fresh tea leaves, and Z-3-hexenol, E-2-hexenol, and methyl n-heptanoate were detected in Jeju dry tea leaves. On the other hand, Z-linalool oxide and myrcene were found in Jeonnam dry tea leaves. The SPME-GC method showed high reproducibility (RSD, 7.4%) with no-artifact formation. In this study, optimum plucking period of tea leaves could be determined for production of high quality green tea with a well-balanced aroma and characteristic VCs in green tea according to growing areas.

Characterization of the Aroma of Salt-fermented Anchovy Sauce Using Solid Phase Microextraction-Gas Chromatography-Olfactometry Based on Sample Dilution Analysis

  • Kim, Hyung-Joo;Baek, Hyung-Hee
    • Food Science and Biotechnology
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    • v.14 no.2
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    • pp.238-241
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    • 2005
  • Aroma-active compounds were evaluated from salt-fermented anchovy sauce by solid phase microextraction-gas chromatography-olfactometry (SPME-GC-O) based on sample dilution analysis (SDA). SPME extract from carboxen/polydimethylsiloxane (CAR/PDMS) fiber was the most similar to the original odor of salt-fermented anchovy sauce used for this experiment, followed by divinylbenzene/CAR/PDMS (DVB/CAR/PDMS) fiber. Because salt-fermented anchovy sauce contains 23% NaCl, NaCl concentration of diluent was considered when salt-fermented anchovy sauce was serially diluted. Linear relationship between GC response and sample concentration was observed when diluted with 23% NaCl solution, whereas not observed when diluted with deodorized distilled water. Eleven and 16 aroma-active compounds were detected by SPME-GC-O based on SDA using CAR/PDMS and DVB/CAR/PDMS fibers, respectively. Butanoic acid and 3-methyl butanoic acid showed the highest ${\log}_2SD$ factors for CAR/PDMS and DVB/CAR/PDMS fibers. Dimethyl trisulfide, methional, trimethyl amine, 1-penten-3-ol, and acetic acid were also detected as potent aroma-active compounds.

Composition of volatile organic components on ballpoint pen inks by HS-SPME GC/MS (HS-SPME GC/MS를 이용한 볼펜잉크의 휘발성 성분 분석)

  • Choi, Mi-Jung;Kim, Chang-Seong;Sun, Yale-Shik;Park, Sung-Woo
    • Analytical Science and Technology
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    • v.23 no.4
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    • pp.414-422
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    • 2010
  • In forensic examinations of question document, analysis about inks components and the dating of ink entries is often of considerable importance and forensic examination of inks is principally concerned with the classification and comparison of chemically complex mixtures. The authenticity about inks analysis of a questioned document may be examined through the analysis of inks used to TLC, HPLC/MS, GC/MS, LDI/MS. We collected 56 difference types of black ballpoint pen inks manufactured from 5 country groups. We identified major 6 species volatile organic components (VOCs), ethylbenzene ($0.089-0.244\;{\mu}g$/mL), o-xylene ($0.072-0.331\;{\mu}g$/mL), m,p-xylene ($0.062-0.318\;{\mu}g$/mL), benzene ($0.003-0.173\;{\mu}g$/mL), 1,1-dichloroethylene ($0.003-0.295\;{\mu}g$/mL), toluene ($0.007-0.484\;{\mu}g$/mL) using HS-SPME GC/MS. The results of this study indicated that determined VOCs of black ballpoint pen inks could make a discriminating tool of inks analysis for forensic question document and can supply methodology for classification and identification of between ballpoints pen inks.

Volatile Compounds of Elsholtzia splendens (꽃향유의 휘발성 향기성분)

  • Lee, So-Young;Chung, Mi-Sook;Kim, Mi-Kyung;Baek, Hyung-Hee;Lee, Mi-Soon
    • Korean Journal of Food Science and Technology
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    • v.37 no.3
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    • pp.339-344
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    • 2005
  • Volatile compounds, isolated from Elsholtzia splendens using simultaneous steam distillation extraction (SDE) and headspace solid phase microextraction (HS-SPME), were analyzed by gas chromatography/mass spectrometry(GC-MS). Twenty-nine compounds, comprising 3 aldehydes, 7 alcohols, 11 hydrocarbons, 5 ketones, and 3 miscellaneous ones, were tentatively identified from volatile compounds of Elsholtzia splendens flowers. From leaves, 30 compounds, comprising 3 aldehydes, 6 alcohols, 11 hydrocarbons, 6 ketones, and 11 miscellaneous ones, were tentatively identified. Volatile compounds extracted by HS-SPME in E. splendens flowers were 3 alcohols, 18 hydrocarbons, 3 ketones, and 2 miscellaneous ones. In leaves, 31 compounds, comprising 7 alcohols, 15 hydrocarbons, 7 ketones, and 2 miscellaneous ones, were tentatively identified. Major volatile compounds identified by SDE and HS-SPME were naginataketone and elsholtziaketone, which were identified as aroma-active compounds, representing characteristic aroma of E. splendens.

Study of the Presence of Residual Hexane in Olive Oils (유통 올리브유의 잔류 헥산에 대한 연구)

  • Kim, Nam-Sook;Lee, Jeung-Hee;Heo, Ok-Soon;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.10
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    • pp.1405-1411
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    • 2006
  • The presence and content of residual hexane in the olive oils were studied. Total 41 olive oils of imported and domestic brands, which were labeled as extra virgin and refined (mixed), were collected from the market. For analysis, electronic nose and headspace SPME-GC/MS were used. Electronic nose equipped with 12 metal oxide sensors was used for the discrimination of odor pattern of olive oils against the different concentrations of hexane. From the results, it is assumed that the contents of residual hexane in the collected olive oils were below 5 ppm. For Qualitative and quantitative analysis of hexane, polydimethylsiloxane (PDMS) fiber was employed for SPME-GC/MS. In the results, the peak of residual hexane was detected in 8 samples from 41 olive oils. But the detected level was no more than 1 ppm that is under the regulation limit (5 ppm) by Korea Food Additive Code.

Determination of VOC in aqueous samples by the combination of headspace (HS) and solid-phase microextraction (SPME) (HS-SPME 방식에 기초한 물 중 VOC 성분의 분석기법에 대한 연구: 3가지 실험 조건의 변화와 분석감도의 관계)

  • Park, Shin-Young;Kim, Ki-Hyun;Yang, H.S.;Ha, Joo-Young;Lee, Ki-Han;Ahn, Ji-Won
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.93-101
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    • 2008
  • The application of solid phase microextraction (SPME) is generally conducted by directly immersing the fiber into the liquid sample or by exposing the fiber in the head space (HS). The extraction temperature, the time of incubation, and application of stirring are often designated to be the most important parameters for achieving the best extraction efficiencies of HS-SPME analysis. In this study, relative importance of these three analytical parameters involved in the HS-SPME method is evaluated using a polydimethylsiloxane/carboxen (PDMS/CAR) fiber. To optimize its operation conditions the competing relationships between different parameters were investigated by comparing the extraction efficiency based on the combination of three parameters and two contracting conditions: (1) heating the sample at 30 vs. 50 C, (2) exposing samples at two durations of 10 vs. 30 min, and (3) application of stirring vs. no stirring. According to our analysis among 8 combination types of HS-SPME method, an extraction condition termed as S50-30 condition ((1) 1200 rpm stirring, (2) $50^{\circ}C$ exposure temp, and (3) 30 min exposure duration) showed maximum recovery rate of 45.5~68.5% relative to an arbitrary reference of direct GC injection. According to this study, the employment of stirring is the most crucial factor to improve extraction efficiency in the application of HS-SPME.

Examination about evaluation method of odor active compounds in evaporator by using condensed water (응축수를 이용한 냉각기의 냄새원인물질 평가방법 검토)

  • Kim, Sun-Hwa;Kim, Kyung-Hwan;Jung, Young-Rim;Kim, Man-Goo;Kim, Jae-Ho;Park, Ha-Young;Ji, Yong-Jun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.361-369
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    • 2007
  • Uncomfortable odor emitted from air conditioning system is the main cause of indoor air quality deterioration. To solve evaporator odor problems, odor active compounds, have to be identified then the quality of the product can be improved its quality. Because evaporator odor in exhaust gas has low odor intensity and discontinuity, it is very difficult to collect and analyze sample. In this study through the identification of odor compounds in condensed water, the evaluation of the eraporator was tested. Odor compounds were extracted from water by headspace-solid-phase microextraction (HS-SPME) method. The single odor was separated by GC/FID/Olfactometry (GC/FID/O) and odor active compounds were identified by GC/AED and GC/MS. Compared to air sample, result of sensory evaluation and the single odor compound appeared similarly. It was identified that odor active compounds have functional group containing oxygen such as alcohols and acids. Evaluation method of odor active compounds using condensed water in evaporator appeared effective on the side of simplicity of collection, low expanse and rapid analysis.

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.

Identification of Irradiation -induced Volatile Marker Compounds in Irradiated Red Pepper Powder (방사선조사 고추가루로부터 휘발성 표지물질의 구명)

  • Kim, Hun;Ahn, Jun-Suck;Sin, Yeong-Min;Lee, Yong-Ja;Lee, Kyung-Hae;Byun, Myung-Woo;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.2
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    • pp.236-242
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    • 2005
  • To develop a new detection method using irradiation-induced volatile marker compounds of red pepper powder (RP), the volatile compounds of irradiated RP (0, 1, 3, 5, and 10 kGy) were analyzed by purge and trap (P&T)/solid phase microextraction (SPME)/gas chromatography/mass spectrometry (GC/MS) methods. A total of 51 and 31 compounds were detected in IRP by SPME and P&T methods, respectively. Among these, 25 compounds, which were composed of 4 hydrocarbons, 7 aldehydes, 1 ketone, 3 alcohols, 4 aromatic compounds, 2 esters and 4 miscellaneous compounds, showed irradiation dependent manner with significant positive correlation (p<0.01 or p<0.05) between irradiation dose and relative concentration. However, all compounds except 1,3-bis(1,1-dimethylethyl)benzene were not suitable as marker compounds because of their low determination coefficients ($R^2$<0.80) between irradiation dose and their concentrations, and detectablilty in nonirradiated sample. Therefore, only one compound, 1,3-bis(1,1-dimethylethyl)benzene, was tentatively identified as a volatile marker compound to detect irradiated RP.