• 제목/요약/키워드: solid phase micro extraction (SPME)

검색결과 43건 처리시간 0.024초

Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
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    • 제34권1호
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    • pp.139-142
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    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

Solid Phase Micro Extraction을 이용한 산초의 휘발성 성분 분석 (Analysis of Volatile Components of Sancho(Zanthoxylum schinifolium)by Solid Phase Micro Extraction)

  • 장희진
    • 한국식품영양학회지
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    • 제12권2호
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    • pp.119-123
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    • 1999
  • Test of the optimum condition of solid phase micro extraction(SPME) was performed by use of 5 vol-atile components in dilute aqueous solution. Volatile components of Sancho(Zanthoxylum schinifolium) were isolated by SPME method and were analyzed by GC/MSD and compared with volatile compone-nts isolated by simultaneous distillation extraction (SDE) method. Total 31 components were identified by comparing gas chromatography retention time and mass spectral data. The major compounds were limonene geranyl acetate $\beta$-phellandrene phellandral mycene linalool rose oxide caproic acid and caprylic acid SPME sampling procedure was found to be a good method for qualitative analysis of the volatile components.

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Dynamic SPME를 이용한 공기 중 지방산 분석 (Analysis of Volatile Fatty Acids in Air by Dynamic SPME)

  • 유미선;양성봉;하남기
    • 한국환경과학회지
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    • 제19권12호
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    • pp.1447-1454
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    • 2010
  • In this study, the detection limits of lower fatty acids in air were investigated by using Dynamic SPME(Solid Phase Micro-Extraction), i.e. improved Head Space - SPME method(HS-SPME). This Dynamic SPME, called SPDE(Solid Phase Dynamic Extraction), is the analytical method for volatile compounds in air with the extraction by using a stainless steel needle of which inner surface is coated with adsorption material and following the gas chromatographic analysis by inserting the needle into a injection port of GC and subsequently, desorption of the volatile compounds into a gas-chromatographic column. Extraction was carried out by passing the sample air through the needle with a suction pump which has been used for a detection tube. The result of measurement for the 6 lower fatty acids showed that the detection limits ranged from 0.10 ppm to 0.44 ppm and the linear correlation coefficients were over 0.99. Relative standard deviations obtained from 5 analytical repetition of a ca. 1.6 ppm standard mixture were in the range of 1.87%~2.47%. This method has been shown to be a adequate for the measuring C2~C5 fatty acids in air in the concentrations of over several hundreds ppb.

Applications of carbon-based materials in solid phase micro-extraction: a review

  • Guo, Jian;Park, Soo-Jin;Meng, Long-Yue;Jin, Xinghua
    • Carbon letters
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    • 제24권
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    • pp.10-17
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    • 2017
  • With continuous development in the field of sample preparation technology, solid phase micro-extraction (SPME) has been widely used in analytical chemistry for high extraction efficiency and convenient operation. Different materials lead to different extraction results. Among existing materials, carbon-based materials are still attracting attention from scientists due to their excellent physical and chemical properties as well as their modifiable surfaces, which could enhance the adsorption effects of SPME fiber. This review introduces the preparation methods and applications of different kinds of carbon-based material coatings on fibers. In addition, directions for future research on carbon material composites are discussed.

A Study on the Analytical Methods Using Solid-phase Extraction for the Determination of Phenols in Water

  • Jeon, Chi-Wan;Lee, Jung-Hwa;Lee, Sang-Hak
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 2003년도 International Symposium on Clean Environment
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    • pp.135-138
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    • 2003
  • Based on solid phase extraction, gas chromatography and mass spectrometry procedure for determining phenol and its derivatives in natural water was presented. In solid phase extraction, three types of techniques using solid phase adsorption material were treated with acid and salt, and converted second portion of acetyl derivatives. Under the these condition, extraction efficiency and detection ability dependent on extraction methods were discussed. Obtained results using optimized solid phase extraction techniques showed more convenience, simplifier and lower cost than the conventional analytical methods with holding wide dynamic range and lower detection limits.

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

  • Cho Tae-Hee;Kang Hee-Gon;Kim Tae-Rang;Chang Min-Su
    • 한국식품위생안전성학회:학술대회논문집
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    • 한국식품위생안전성학회 2001년도 The Asia-Pacific Conference on Reproductive Biology and Environmental Sciences
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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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Absorption of d-Limonene in Orange Juice into a Laminated Food Package Studied with a Solid Phase Micro-extraction Method

  • Lee, Hahn-Bit;Yang, Hee-Jae;Min, Sea-C.
    • 산업식품공학
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    • 제14권4호
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    • pp.354-358
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    • 2010
  • The methods for determining the diffusion parameters for the diffusion of d-limonene, a major volatile compound of orange juice, through a multi-layered food packaging material and predicting its absorption into the packaging material have been investigated. The packaging material used was the 1.5-mm thick multi-layered packaging material composed of high impact polystyrene (HIPS), polyvinylidene chloride (PVDC), and low density polyethylene (LDPE). Orange juice was placed in a cell where volatiles were absorbed in the sample package and kept at $23{\pm}2^{\circ}C$ for 72 hr. The d-limonene absorbed in a 1.5-mm thick multi-layered food packaging material was analyzed by a solid phase micro-extraction (SPME). The absorption parameters for the absorption of d-limonene in the packaging material were determined and absorption of d-limonene into the packaging material was predicted using absorption storage data. The SPME desorption at $60^{\circ}C$ for 1 hr resulted in the most sensitive and reproducible results. The diffusion coefficients of d-limonene in the packaging material and the partition coefficient at $23{\pm}2^{\circ}C$ were approximately $1-2{\times}10^{12}m^2$/s and 0.03, respectively. The absorption profile no earlier than 30 hr was fit well by a model derived from the Fick's law.

고상 미량 추출 장치(SPME, solid phase micro-extraction device)를 이용한 물 중의 THM(trihalomethane) 분석 (Determination of THM(trihalomethane) in Rain by using Solid Phase Micro-Elctraction(SPME) Fiber Assembly)

  • 유광식;박상윤
    • 한국환경과학회지
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    • 제6권3호
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    • pp.277-283
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    • 1997
  • SPME deuce was applied to determine the THM in an aqueous solution. The 6 kinds of THM was quantitatively detenuned by using GC-ECD which has the sample eutracted on the SPME fiber from an aqueous solution for 10 min. The THM components were well separated from $CHCl_3$ to the last $CHBr_3$ UHh 13 mons at the condition. 6 kinds of the volatile halogenated organic compounds: $CHCl_3$, $CHBrCl_2$, $CHBrtCl_2$, $CHCl_3$, $C_2Cl$. and $CHBr_3$, showed well defirled calibration graph with good llnearlty from a few ppb level up to several tens of pub concentration. $CHBr_2Cl$ and $C_2C1_4$ were detected from a few samples among the 10 of river samples. CHCl3, however, was detected In 4 sea water samples with the highest of 10 ppd among the pouuted 6 positions. Trace level of $CHBr_2Cl$ and few pub level of $CHBr_3$ were also detected at the other two sample stations. Most of the 13 rain water samples collected from 6 sampling stations were contained ppd level of $CHCl_3$, and also $CHBr_2Cl$, and C_2Cl_4$ were only detected at trace level at a few rain samples among them. We could recognize the fact that our Ut and water enoronment has already been contaminated by certain volatile halogenated organic compounds through this study.

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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.