• 제목/요약/키워드: solid-phase microextraction (SPME)

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Solid-Phase Microextraction (SPME)에 의한 꿀풀과 약초의 향기성분과 그 특성 (Volatile Aroma Compounds and Their Characteristics of Labiatae by Solid-Phase Microextraction (SPME))

  • 송영은;구창섭;문성필;류지성;김대향;최정식;최영근
    • 한국약용작물학회지
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    • 제10권2호
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    • pp.120-125
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    • 2002
  • 본 연구는 향기성분을 많이 포함하고 있는 꿀풀과의 대표적인 5종류를 선정하여 이들을 대상으로 소량의 시료만으로도 신속하게 분석할 수 있는 고상 미량 추출법(Solid Phase Microextraction: SPME)과 동시증류추출법(Simultaneous Distillation and Extraction : SDE)으로 향기성분을 분석하였다. 분석결과 5종류의 꿀풀과 약초의 향기성분 구성은 linanol, limonene, citral, trans-geraniol 등의 monoterpene alcohol, monoterpene aldehyde 및 ketone 과 trans-caryophyllene, ${\delta}-cadinene$ 등의 sesquiterpene 성분들이 주로 검출되었다. 분석결과 기존의 향기성분 연구에 많이 사용되는 동시증류추출법(SDE)과 주성분에서 대부분 유사하였으나 형개의 향기성분처럼 SPME법에서 많은 성분이 검출되지 않는 경우도 있었고 배초향, 박하의 성분처럼 SDE법에서 검출되지 않은 일부 성분도 SPME법에서 검출되기도 하였다. 이러한 결과는 SPME법은 낮은 온도에서 흡착만으로 성분의 포집이 이루어지므로 추출, 농축 등의 조작에 의한 SDE법보다 이차적인 변질이 적었기 때문으로 생각되었다. 따라서 SPME법은 열변성이 적고 소량으로 다수의 시료를 분석할 수 있어 향신약초의 품종육종 등에 사용할 수 있는 간편하고 신속한 방법이 될 것으로 생각된다.

Solid Phase Microextraction 및 Purge & Trap을 이용한 생물시료 중 휘발성 유기화합물의 GC/MS 분석비교 (Comparison Solid Phase Microextraction with Purge & Trap on the GC/MS Analysis of Volatile Organic Compounds in Biota Samples)

  • 안윤경;서종복;홍종기
    • 분석과학
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    • 제14권5호
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    • pp.392-399
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    • 2001
  • 생물시료에 존재하는 휘발성 유기화합물 중 n-butylbenzene과 1,2-dibromo-3-chloropropane (DBCP)를 기체크로마토그래피/질량분석기-선택이온검색법에 의해 수행하였다. 시료 중 휘발성 유기화합물은 $100{\mu}m$ polydimethyl siloxane (PDMS) fiber를 사용하여 headspace solid phase microextractio (SPME) 및 purge & trap 방법에 의해 추출 및 비교하였다. SPME에 의한 회수율은 n-butylbenzene의 경우 85.8%, DBCP의 경우 92.4%로 나타났고 검출한계는 각각 $0.15{\mu}g/kg$, $0.05{\mu}g/kg$로 나타났다. 반면, purge & trap의 경우 회수율은 n-butylbenzene의 경우 115.2%, DBCP의 경우는 80.9%로 나타났고 검출한계는 각각 $0.04{\mu}g/kg$$0.70{\mu}g/kg$로 나타나 두 방법에 있어 국내에서 규제하는 검출한계측면에서 큰 차이는 없었다.

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Static headspace, purge & trap 및 solid-phase microextraction을 이용한 시판우유의 휘발성 향기성분 분석 (Volatile Flavor Compounds in Commercial Milk by Static Headspace, Purge and Trap, Solid-Phase Microextraction)

  • 이홍민;이기웅;장치훈;김성한
    • 한국식품과학회지
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    • 제38권6호
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    • pp.738-741
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    • 2006
  • 본 실험에서는 시판중인 우유 4종을 대상으로 static headspace, purge and trap 및 SPME의 세 가지 향기성분 추출방법을 이용하여, GC/MS로 각각의 향기성분을 분석하였다. Purge and trap법을 이용한 분석법으로 가장 많은 종류의 성분을 분석할 수 있었으며, 향기성분의 추출효율이 가장 좋았다. SPME법은 간단한 장비로 신속하게 향기성분을 포집할 수 있는 장점이 있으며, 추출 효율 또한 뛰어나 효율적인 향기성분 분석방법으로 이용이 가능하였다. 4종의 시판우유 중에서 검출된 향기성분은 대체적으로 큰 차이를 나타내지 않았으나, 다소의 양적차이를 나타내었다. 검출 된 성분은 주로 acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone 등의 케톤류, pentanal, 2-methylbutanal, hexanal, benzaldehyde 등의 알데하이류 및 dimethyl sulfide 등의 황화합물류로써, 우유의 주요 이취성분들이었다.

Headspace법에 의한 솔향의 분석 (Comparisons of Volatile Compounds Extracted from Pinus densiflora by Headspace Analysis)

  • 이미정;정은주;이신조;조지은;이양봉;조현종;윤정로
    • 한국식품영양과학회지
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    • 제31권1호
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    • pp.26-31
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    • 2002
  • Pinus densiflora(2엽송) 1년생을 채취하여 가지, 잎, 새순 부분으로 구분하고, 시료병에 넣어 밀봉한 뒤, solide phase microextraction (SPME)과 dynamic headspace analysis(DHA)를 이용하여 휘발성 성분을 분리, 동정하였다. SPME와 DHA의 결과를 terpenes의 구성 성분에 따라 monoterpenes과 sesquiterpenes, oxygenated terpenes으로 나누어 조성비를 살펴보면, monoterpenes의 조성은 잎의 경우 각각 66.7%와 14.3%, 새순은 90.6%와 0.7%, 가지에서는 90.6%와 1.2%로 나타났다. Sesquiterpenes의 함량은 SPMe의 결과에서만, 잎이 25.8%, 가지 4.4%, 새순 1.5%로 나타났다. 산소를 함유하고 있는 terpenes의 함량은 새순 부위가 4.7%, 79.0%로 나타났으며, 가지 부위는 3.7%와 70.4%, 잎에서 1.0%와 50.7%를 각각 차지하였다. SPME의 결과는 이전의 용매추출을 통한 결과와 다소 비슷한 양상을 보였으며, DHA의 결과는 10$0^{\circ}C$이상의 고비점 화합물들이 나타나지 않은 반면, 5$0^{\circ}C$이하의 저비점 화합물이 15개 분리되었다.

The Evaluation of Solid-Phase Microextraction(SPME) Techniques for Analyzing Mixed Fuel Oxygenates and Products

  • 이재선;이시진;장순웅
    • 한국지하수토양환경학회:학술대회논문집
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    • 한국지하수토양환경학회 2003년도 추계학술발표회
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    • pp.458-461
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    • 2003
  • Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

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Optimization of Headspace Sampling Using Solid Phase Microextraction For Volatile Organic Acids in Different Tobacco Types

  • Lee, Jang-Mi;Lee, Jeong-Min;Son, Seong-Ae;Kwon, Young-Ju;Jang, Gi-Chui;Kim, Young-Ho
    • 한국연초학회지
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    • 제35권1호
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    • pp.7-12
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    • 2013
  • A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.

Determination of Acrylamide in Foods by Solid Phase Microextraction-Gas Chromatography

  • Chen, Liangbi;Liu, Haizhu;Yu, Ping;Zhao, Jinyun;Chen, Xi
    • Food Science and Biotechnology
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    • 제18권4호
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    • pp.895-899
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    • 2009
  • A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.

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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    • 제14권2호
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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.

Nerve Agents and Their Detection

  • Kim, Young Jun;Huh, Jae Doo
    • 센서학회지
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    • 제23권4호
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    • pp.217-223
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    • 2014
  • Nerve agents are major chemical warfare agents with the "G series" and "V series" being the most widely known because of their lethal effect. Although not conspicuously used in major wars, the potential detrimental impact on modern society had been revealed from the sarin terror attack on Tokyo subway, which affected thousands of people. In this mini-review, major nerve agents of the "G series" and "V series" have been described along with various types of their detection methods. The physical properties and hydrolysis mechanisms of the major nerve agents are discussed since these are important factors to be considered in choosing detection methods, and specifying the procedures for sample preparations in order to enhance detection precision. Various types of extraction methods, including liquid-phase, solid-phase, gas-phase and solid-phase microextraction (SPME), are described. Recent development in the use of gas sensors for detecting nerve agents is also summarized.