• 제목/요약/키워드: GC-SPME

검색결과 220건 처리시간 0.027초

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

  • 조덕희
    • 상하수도학회지
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    • 제18권5호
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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.

Analysis of Fragrance Volatiles of Korean Rosa hybrida Using Gas Chromatography-Mass Spectrometry

  • Cho, Yong-Sik;Cho, In-Hee;Park, Hong-Ju;Chun, Hye-Kyung
    • Journal of Applied Biological Chemistry
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    • 제49권4호
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    • pp.180-185
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    • 2006
  • Two different extraction procedures, SDE and SPME, were employed to determine a comprehensive and efficient fragrance profile of Korean Rosa hybrida. Both extraction methods could compensate for each other, covering compounds with diverse boiling point, polarities, and chemical properties. A total of 46 compounds were identified in Mi-hyang. The identified compounds were composed of 17 alcohols, 14 carbonyls, 7 aliphatic hydrocarbons, 2 terpene hydrocarbons, 4 benzenes, 1 ester, and 1 miscellaneous compound. Quantitatively, carbonyls($12.96{\sim}21.79%$ in essential oils of SDE and $2.89{\sim}8.44%$ in SPME headspace) and alcohols($7.98{\sim}11.73%$ in essential oils of SDE and $3.39{\sim}17.35%$ in SPME headspace) were dominant in Mi-hyang's volatiles.

물중의 잔류농약 분석을 위한 SPME의 최적조건 선정에 관한 연구 (Preparation of Optimal Condition for Residual Pesticides Analysis by Solid-Phase Microextraction in Water)

  • 장미라;정효준;이홍근
    • 한국물환경학회지
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    • 제18권4호
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    • pp.421-433
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    • 2002
  • This study was conducted to develope a simple, rapid and solvent-free solid-phase microextraction(SPME) procedure for extracting three organochlorine, one triazine and nine organophosphorus pesticides from water. The optimal conditions of SPME for analyses of organochlorine pesticides were obtained at $250^{\circ}C$ of desorption temperature, 45 minutes of equilibrium time, pH 6 and NaCl 0% addition using $100{\mu}m$ polydimethylsiloxane fiber and those of triazine and organophosphorus pesticides were obtained at $270^{\circ}C$ of desorption temperature, 60 minutes of equilibrium time, pH 6 and NaCl 0% addition using $100{\mu}m$ polydimethylsiloxane fiber. This method showed good lineality for organochlorine pesticides between 0.0001 and $10{\mu}g/L$ with regression coefficients ranging 0.9986~0.9992 and for triazine and organophosphorus pesticides between 0.01 and $10{\mu}g/L$ with regression coefficients ranging 0.9867~0.9998.

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
    • 한국연초학회지
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    • 제30권2호
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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.

고상 미세 추출법을 이용한 가스시료 중 휘발성유기화합물의 정량 분석 (Quantification of Volatile Organic Compounds in Gas Sample Using Headspace Solid-Phase Microextraction)

  • 김재혁;김현욱
    • 대한환경공학회지
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    • 제35권12호
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    • pp.906-917
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    • 2013
  • 본 연구에서는 고상 미세추출법(HS-SPME)을 적용하여 대기환경시료 중 VOCs 분석을 위한 응용성을 평가하고자 하였다. 광범위한 VOCs 검출을 위한 최적 HS-SPME 분석 조건(CAR/PDMS fiber, 30분 시료노출, 도출된 분석조건)에서 VOCs의 검출 한계 농도는 저분자량 화합물인 경우 1~3 ppbv 내외였고, BTEXs 계열 화합물들의 경우에는 0.0005 ppbv 이하의 매우 낮은 농도까지 검출 가능하였다. 다만 fiber들 간의 흡착효율 재현성 평가결과, 동일 fiber에 대하여 1~9.2% (n = 3), 서로 다른 fiber들에 대하여서는 5.9~13.5% (n = 5)의 오차를 보였다. 도출된 분석조건을 이용하여 매립지 가스 중 BTEX를 포함한 35여종의 VOCs를 성공적으로 정량분석하였다.

SPME에 의한 소엽의 향기성분 분석 (Analysis of Volatile Compounds in Perilla frutescens var. acuta by Solid Phase Microextraction)

  • 정미숙;이미순
    • 한국식생활문화학회지
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    • 제18권1호
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    • pp.69-74
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    • 2003
  • 우리나라의 고유한 향신료로 활용되고 있는 소엽의 휘발성 향기성분 분석에 적합한 solid phase microextraction(SPME) fiber를 선정하기 위하여 carboxen/polydimethylsiloxane(CAR/PDMS)과 polydimethylsiloxane(PDMS)의 2종류 fiber를 이용하여 향을 추출한 후 GC/MS로 분석하였다. CAR/PDMS fber에 소엽의 향을 흡착시켜 분석한 결과, 39종의 성분이 확인되었으며, PDMS fiber를 이용하였을 때는 20가지의 향기성분이 확인되었다. 특히 PDMS fiber를 사용하였을 때 CAR/PDMS fber를 이용하였을 때 보다 perillaldehyde (40.50%), limonene (27.32%), E,E-,${\alpha}-famesene$ (10.22%) 및 ${\beta}-caryophyllene$ (8.02%)의 소엽의 주요 향기성분이 선택적으로 많이 확인되었다. 따라서 방향성 식용식물인 소엽의 향기를 SPME법으로 추출할 때는 PDMS fiber가 적합하다고 판단된다.

추출방법에 따른 잎담배 종류별 휘발성 향기성분 특성비교 (Comparison of the volatile flavor compounds in different tobacco types by different extraction methods)

  • 이장미;이정민;이창국;복진영;황건중
    • 한국연초학회지
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    • 제32권2호
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    • pp.77-87
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    • 2010
  • Traditional simultaneous distillation extraction(SDE) and solid-phase micro extraction(SPME) methods using GC/MS were compared for their effectiveness in the extraction of volatile flavor compounds from different tobacco leaves types(flue-cured, burley, oriental). The major volatile flavor compounds of flue-cured and burley tobacco were similar such as neophytadiene, solanone, megastigmatrienone isomers, ${\beta}$-damascenone and ${\beta}$-ionone. On the other hand, volatile flavor compounds such as norambreinolide, sclareolide were specifically identified in oriental tobacco. Each method was used to evaluate the responses of some analytes from real samples and standards in order to provide sensitivity comparisons between two techniques. Among three types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate) and PDMS/DVB (Polydimethylsiloxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency, PDMS/DVB fiber was selected for the extractions of the volatile flavor compounds due to its effectiveness. The qualitative analysis showed that the total amount of volatile flavor compounds in SDE method(130 species) was much more than that in SPME method(85 species). SPME method was more efficient for all the highly volatile compounds than SDE method, but on the other hand, low-volatile compounds such as fatty acids or high-molecular hydrocabons were detected in SDE method. SPME method based on a short-time sampling can be adjusted to favor a selected group compounds in tobacco. Furthermore this results could be used to estimate the aroma characteristics of cigarette blending by using a different type of tobacco with more effectiveness and convenience.