• Title/Summary/Keyword: solid phase microextraction (SPME)

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

  • Chung, Mi-Sook;Lee, Mie-Soon
    • Journal of the Korean Society of Food Culture
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    • v.18 no.1
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    • pp.69-74
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    • 2003
  • This study was conducted to find the appropriate fiber for extraction of volatile compounds from Perilla frutescens var. acuta. by solid phase microextraction (SPME). Two SPME fiber, carboxen/polydimethylsiloxane (CAR/PDMS) and polydimethylsiloxane (PDMS) were used to determine the selectivity of the fibers to the different flavor compounds present in the Perilla frutescens var. acuta. Thirty-nine compounds were identified in the volatile compounds extracted by CAR/PDMS fiber, including 6 aldehyde, 1 alcohol, 10 hydrocarbons, 17 terpene hydrocarbons, 2 ketones and 3 benzenes. In PDMS fiber, 3 aldehydes, 2 alcohols, 13 terpene hydrocarbons and 2 miscellaneouses were identified. Perillaldehyde was found to be major volatile flavor component of fresh Perilla frutescens var. acuta. Perillaldehyde and terpene hydrocarbons were more identified in PDMS fiber. These results suggested that the selectivity of PDMS fiber was better than that of CAR/PDMS fiber in Perilla frutescens var. acuta..

Analysis of Trace Levels of Halonitromethanes (HNM) in Water using Headspace-SPME and GC-ECD (Headspace-SPME와 GC-ECD를 이용한 수중의 미량 Halonitromethane (HNM)류 분석)

  • Kang, So-Won;Son, Hee-Jong;Seo, Chang-Dong;Kim, Kyung-A;Choi, Jin-Taek
    • Journal of Korean Society of Environmental Engineers
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    • v.37 no.5
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    • pp.293-302
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    • 2015
  • Halonitromethanes (HNMs) are one of the most toxic groups of disinfection by-products. Recently, various studies have been fulfilled. An automated headspace-solid phase microextraction (SPME) gas chromatography/electron capture detector (GC-ECD) technique was developed for routine analysis of 9 HNMs in water samples. The optimization of the method is discussed. The limits of detection (LOD) and limits of quantification (LOQ) range from 90 ng/L to 260 ng/L and from 270 ng/L to 840 ng/L for 9 HNMs, respectively. Matrix effects in tap water and sea water were investigated and it was shown that the method is suitable for the analysis of trace levels of HNMs, in a wide range of waters. The method developed in the present study has the advantage of being rapid, simple and sensitive.

Determination of Volatile Fatty Acids in Aqueous Samples by HS-SPME with In-Fiber Derivatization (Fiber내 유도체화/HS-SPME를 이용한 수용액 시료 중 휘발성 지방산의 분석)

  • Ahn, Yun Gyong;Lee, Jee Yeon;Kim, Jeehyeong;Hong, Jongki
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.458-465
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    • 2003
  • The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

Comparison of Solid Phase Microextraction-Gas Chromatograph/Pulsed Flame Photometric Detector (SPME-GC/PFPD) and Static Headspace-Gas Chromatograph/Pulsed Flame Photometric Detector (SH-GC/PEPD) for the Analysis of Sulfur-Containing Compounds (Solid phase microextraction-gas chromatograph/pulsed flame photometric detector(SPME-GC/PFPD)와 static headspace-gas chromatograph/pulsed flame photometric detector(SH-GC/PEPD)를 이용한 황 함유 화합물들의 분석 방법 비교)

  • Yang, Ji-Yeon;Kim, Young-Suk
    • Korean Journal of Food Science and Technology
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    • v.37 no.5
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    • pp.695-701
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    • 2005
  • Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

Simultaneous Determination of Phthalates(DMP, DEP, DBP, BBP, DEHP, DnOP) by Solid Phase Microextraction-GC/MS (Solid Phase Microextraction-GC/MS에 의한 플라스틱가소제(DMP, DEP, DBP, BBP, DEHP, DnOP)의 동시분석)

  • Lee, Jae-Hee;Bae, Jun-Hyun;Kang, Jun-Gill;Kim, Youn-Doo
    • Journal of the Korean Chemical Society
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    • v.48 no.1
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    • pp.17-27
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    • 2004
  • A procedure based on solid phase microextraction extraction(SPME)-GC/MS has been developed for the simultaneous analysis of plasticizers. The plasticizers investigated in this study are dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP), benzylbutyl phthalate(BBP), diethylhexyl phthalate (DEHP), di-n-octyl phthalate(DnOP). The limit of detection(LOD) was 0.163~0.299 with relative standard deciation(RSD) of 5.85~15.80% for these compounds. At water reserviors of Han, Geum, Nakdong and Sumjin rivers, only DBPand DEHP were detected at trace level, 0.192~1.270 ng/ml for DBP and 0.077~1.102 ng/ml for DEHP depending on the river.

Comparison of Volatile Flavor Compounds in Meat of the Blue Crab Using V-SDE and SPME Methods (V-SDE와 SPME법에 의한 꽃게(Portunus trituberculatus)육의 휘발성 향기성분 비교)

  • Cha, Yong-Jun;Cho, Woo-Jin;Jeong, Eun-Jeong
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.6
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    • pp.441-446
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    • 2006
  • Volatile flavor compounds in meat of the blue crab Portunus trituberculatus were compared using vacuum simultaneous steam distillation-solvent extraction (V-SDE) and solid phase microextraction (SPME)/ gas chromatography (GC)/ mass selective detection (MSD) methods. A total of 100 volatile flavor compounds were identified by both methods: 77 by V-SDE and 59 by SPME. These compounds were composed of 17 aldehydes, 12 ketones, 19 alcohols, 5 esters, 4 sulfur-containing compounds, 6 nitrogen-containing compounds, 23 aromatic compounds, 6 hydrocarbons, 2 terpenes, and 6 miscellaneous compounds. Although more compounds were detected using V-SDE than using SPME, the levels of all groups detected, except esters, were higher using SPME than using V-SDE. In addition to trimethylamine, aldehydes, and aromatic compounds, the S- and N-containing compounds with low thresholds are thought to have positive roles for flavors in the meat of the blue crab.

Determination of DBCP and n-Butylbenzene using SPME with GC-MS (SPME-GC-MS를 이용한 DBCP 및 n-Butylbenzene의 분석)

  • Park, Hyun-Mee;Kim, Young-Man;Lee, Dai-Woon;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.471-475
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    • 2001
  • Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

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Volatile Component of Pine Needles from Pinus densiflora S. using Solid Phase Microextraction-Ges Chromatography-Mass Spectrometry

  • Lee Jae-Gon;Lee Chang-Gook;Back Shin;Jang Hee-Jin;Kwag Jae-Jin;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.18 no.4
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    • pp.373-379
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    • 2005
  • The volatile components of Pinus densiflora needles were studied by gas chromatography-mass spectrometry(GC-MS), using seven kinds of solid phase microextraction (SPME) fibers, seven in SPME fibers: 100 ${\mu}m$ PDMS, 65 ${\mu}m$ PDMS/DVB, 65 ${\mu}m$ SF-PDMS/DVB, 85 ${\mu}m$ PA, 75 ${\mu}m$ CAR/PDMS, 65 ${\mu}m$ CW/DVB and 50/30 ${\mu}m$ DVB/CAR/PDMS fibers. A total of 40 components were identified by using the seven different SPME fibers. The identified components were classified, according to their functionalities, as follows: 26 hydro-carbons, 7 alcohols, 4 carbonyl compounds, and 3 esters. The major volatile components of Pinus densiflora needles identified by these SPME fibers were $\alpha$-pinene ($1.7\~21.7\;{\mu}g/g$), $\beta$-myrcene ($2.0\~20.1\;{\mu}g/g$), $\beta$-phel-landrene ($4.6\~22.8\;{\mu}g/g$), $\beta$-caryophyllene ($6.7\~26.0\;{\mu}g/g$) germacrene D ($1.1\~11.9\;{\mu}g/g$). In the comparison of the seven SPME fibers, PDMS appeared to be the most suitable fiber for the analysis of hydrocarbon compounds and CAR/DPMS, PDMS/DVB, CW/VB and DVB/CAR/PDMS are shown to be optimal for analysis of the alcohols and carbonyl compounds.

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.