• Title/Summary/Keyword: SPME

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Determination of Volatile Organic Compounds (VOCs) Using Tedlar Bag/Solid-phase Microextraction/Gas Chromatography/Mass Spectrometry (SPME/GC/MS) in Ambient and Workplace Air

  • Lee, Jae-Hwan;Hwang, Seung-Man;Lee, Dai-Woon;Heo, Gwi-Suk
    • Bulletin of the Korean Chemical Society
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    • v.23 no.3
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    • pp.488-496
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    • 2002
  • SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

Wound-State Monitoring for Burn Patients Using E-Nose/SPME System

  • Byun, Hyung-Gi;Persaud, Krishna C.;Pisanelli, Anna Maria
    • ETRI Journal
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    • v.32 no.3
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    • pp.440-446
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    • 2010
  • Array-based gas sensors now offer the potential of a robust analytical approach to odor measurement for medical use. We are developing a fast reliable method for detection of microbial infection by monitoring the headspace from the infected wound. In this paper, we present initial results obtained from wound-state monitoring for burn patients using an electronic nose incorporating an automated solid-phase microextraction (SPME) desorption system to enable the system to be used for clinical validation. SPME preconcentration is used for sampling of the headspace air and the response of the sensor module to variable concentrations of volatiles emitted from SPME fiber is evaluated. Gas chromatography-mass spectrometry studies prove that living bacteria, the typical infectious agents in clinical practice, can be distinguished from each other by means of a limited set of key volatile products. Principal component analysis results give the first indication that infected patients may be distinguished from uninfected patients. Microbial laboratory analysis using clinical samples verifies the performance of the system.

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

  • 이재선;이시진;장순웅
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.09a
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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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Analysis of 111 VOCs using SPME-GC/MS (SPME-GC/MS에 의한 111종 VOCs 분석법 확립)

  • 김대원;허귀석;유혜경;홍진희
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2001.11a
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    • pp.344-345
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    • 2001
  • 대기 중에는 ppb 수준의 매우 미량으로 많은 VOC 성분이 존재하고 있어 이를 효과적으로 신속하고 적은 비용으로 분석할 수 있는 분석할 필요성이 커지고 있다. 그러므로, 본 연구에서는 대기중의 VOC성분을 SPME-GC/MS법을 이용하여 효율적으로 분석하기 위한 분석법을 개발하고자 하였다. 유해성이 큰 halocarbon, aromatic, haloaromatic V()Cs 42 종(USEPA TO-14)과, 오존을 유발시키는 오존전구물질 VOCs 53 종, 국내 규제 VOCs 33종, 그리고 악취물질(국내 8종 포함 일본 악취물질 22종)을 전부 포함하는 111종의 VOC를 SPME-GC/MS를 이용하여 신속하게 정성, 정량분석할 수 있는 방법을 확립하고저 하였다. (중략)

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SPME-GC/MS와 전자코(Electronic Nose)를 이용한 재래흑돼지와 개량종 돼지 가열육의 휘발성 향기 성분 및 향기 패턴 비교

  • Gang, Seon-Mun;Lee, Seong-Gi
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2006.05a
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    • pp.209-213
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    • 2006
  • 본 연구는 재래흑돼지와 개량종 돼지 가열육의 SPME-GC/MS와 전자코를 이용한 휘발성 향기 성분 및 향기 패턴 비교를 구명하고자 실시하였으며, 평균 생시 체중이 70 kg인 재래흑돼지(거세돈) 5두와 103 kg인 개량종 돼지($Landrace{\times}Yorkshire$,거세돈) 5두를 도축후 뒷다리 부위를 시료로 이용하였다. SPME-GC/MS를 이용한 휘발성 향기 성분에서 6-mehtyl-1-heptanol이 재래흑돼지육에서만 검출되었고, 1-octen-3-ol과 benzaldehyde가 재래흑돼지육이 개량종 돼지육보다 유의적으로 높았다(p<0.05). 전자코의 PCA에 의한 향기 패턴은 두 품종간에 큰 차이를 보이지 않았다. 따라서 재래흑돼지 가열육이 개량종 돼지 가열육보다 높은 6-mehtyl-1-heptanol, 1-octen-3-ol, benzaldehyde를 가졌으며, SPME-GC/MS와 전자코에 의해 품종이 다른 가열 돈육의 휘발성 향기 성분과 패턴을 성공적으로 분별하였다.

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Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Comparison on Usefulness of Sampling Methods of Indoles in Airs from Swine Facility by Tenax-TA and SPME

  • Yu, Mee-Seon;Lee, Jae-Chun;Yang, Sung-Bong;Kim, Doo-Hwan;Cho, Sung-Back;Whang, Ok-Wha
    • Journal of Environmental Science International
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    • v.22 no.12
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    • pp.1539-1549
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    • 2013
  • The purpose of this study is to compare the sampling methods for monitoring indoles (phenol, p-cresol, indole and skatole) in airs of swine facility. As the collecting methods of indoles in air, Tenax-TA adsorption tube and solid phase microextraction (SPME) were examined. For the preparation of calibration curves of indoles concentrated in Tenax-TA, the standard indoles solutions were spiked in each of Tenax-TA tubes and thermally desorbed (ATD) into a gas chromatograph combined with mass detector (GC/MS). And for the preparation of calibration curves by SPME, indoles in the standard gaseous solution prepared by evaporating the aqueous solution that contained indoles into a polyester sampling bag were extracted with SPME fiber and subsequently analyzed by the GC/MS. Two sampling methods were evaluated for extracting indoles present in swine building environments. Results indicated that the SPME method using Polydimethylsiloxane/ Divinylbenzene (PDMS/DVB) fiber was more effective than Tenax-TA method in extracting indoles. The gas chromatographic analysis showed that the linearities of calibration curves and detection limits were useful for detection of indoles in swine airs. The field tests also showed that considerably different levels of indoles were present in various parts of the swine building.

Application of Solid Phase Microextraction to the Analysis of Pesticides in Vegetables

  • Cho Tae-Hee;Kang Hee-Gon;Kim Tae-Rang;Chang Min-Su
    • Proceedings of the Korean Society of Food Hygiene and Safety Conference
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    • 2001.10a
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    • pp.171-174
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    • 2001
  • Solid phase micro-extraction (SPME), a solvent-free, rapid and inexpensive method for the extraction of organic compounds from aqueous sample matrices, was evaluated for determination of the 120 pesticides in vegetables such as crown daisy, perilla leaf, leafy lettuce and to mato. The analysis conditions were chosen for the SPME method: 15 min of immersion of the PDMS fiber in 10 ml of the solution with stirring at 1,000 rpm. The recovery tests were carried out in triplicate. The range of recoveries was 0-142% for organochlorine pesticides and $4.9\sim200\%$ for organophosphorus pesticides. The recoveries were very low in the pesticide groups with low solubility in water. The recoveries became lower in proportion to the interference materials in vegetables. The recovery in tomato was relatively higher than that in perilla Ie af and crown daisy. The recovery values obtained by SPE and SPME were compared. In leaf y lettuce, recovery obtained by SPE method ranged from $58.1\%\;to\;136.1\%$ and recovery by SPME ranged from $9.6\%\;to\;176.3\%$ In organophosphorus pesticides. The recovery in SPME method was satisfactory with $136\%$ for ethoprophos, $119\%$ for methidathion and $113\%$ for diazinon. Meanwhile, recovery of EPN, phenthoate and 2,4-DDT revealed relatively low value of $38\%,\;41\%\;and\;3.4\%,$ respectively. However, most of pesticides applied to SPME method sho wed constant recovery and precision. From these results, it can be concluded that solid phase micro-extraction might be an appropriate method for the screening test of pesticides in vegetables.

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

  • Ahn, Yun-Gyong;Seo, Jong-Bok;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.392-399
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    • 2001
  • The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

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Aroma Characteristic of Chungkukjang with Astragalus membranaceus (황기청국장의 향기특성)

  • Yoon Hyang-Sik;Choi Hye-Sun;Joo Seon-Jong;Kim Ki-Sik;Kim Sook-Jeong
    • Food Science and Preservation
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    • v.13 no.2
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    • pp.269-272
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    • 2006
  • Aroma compounds in chungkukjang with Astragalus membranaceus (Hwangki) were extracted by the simultaneous distillation and extraction (SDE), headspace and solid phase microextraction (SPME), and aroma compounds obtained by this method were identified with GC-MS. Thirty compounds were identified, including six ketones, eight alcohols, three heterocyclic compounds, three aldehydes, five hydrocarbones and five other compounds. Major aroma compounds were identified as 3-hydroxy-2-butanone, 2-furanmethanol, 2-methoxy-4-vinylphenol, and 4-vinylphenol in SDE, 2,3-butanedione, 3-hydroxy-2-butanone, ethanol, 2,6-dimethyl pyrazine and acetic acid in headspace and acetone, ethanol, 2,5-dimethyl pyrazine, tetramethyl pyrazine and acetic acid in SPME. The content of pyrazines identified in headspace and SPME methods was higher than that of SDE method, and the content of pyrazines containing 2,5-dimethyl pyrazine, 2,6-dimethyl pyrazine and tetramethyl pyrazine in chungkukjang was higher than that of Hwangki chungkukjang.