• Title/Summary/Keyword: Micro solid phase extraction

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

  • 장희진
    • The Korean Journal of Food And Nutrition
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    • v.12 no.2
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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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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
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2003.11a
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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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On-Channel Micro-Solid Phase Extraction Bed Based on 1-Dodecanethiol Self-Assembly on Gold-Deposited Colloidal Silica Packing on a Capillary Electrochromatographic Microchip

  • Park, Jongman;Kim, Shinseon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.45-50
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    • 2014
  • A fully packed capillary electrochromatographic (CEC) microchip with an on-column micro-solid phase extraction (SPE) bed for the preconcentration and separation of organic analytes was prepared. A linear microchannel with monodisperse colloidal silica packing was formed on a cyclic olefinic copolymer microchip with two reservoirs on both ends. Silver-cemented silica packing frit structure was formed at the entrance of the microchannel by electroless plating treatment as a base layer. A gold coating was formed on it by reducing $Au^{3+}$ to gold with hydroxylamine. Finally micro-SPE bed was formed by self-assembly adsorption of 1-dodecanethiol on it. Micro-SPE beds were about 100-150 ${\mu}m$ long. Approximately $10^3$ fold sensitivity enhancements for Sulforhodamine B, and Fluorescein in nM concentration levels were possible with 80 s preconcentration. Basic extraction characteristics were studied.

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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    • v.34 no.1
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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).

Analysis of Flavor Composition of Coriander Seeds by Headspace Mulberry Paper Bag Micro-Solid Phase Extraction

  • Cha, Eun-Ju;Won, Mi-Mi;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2675-2679
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    • 2009
  • This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

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.
    • Food Engineering Progress
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    • v.14 no.4
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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.

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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    • v.24
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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.

Mulberry Paper Bag μ-Solid Phase Extraction for the Analysis of Five Spice Flavors by Gas Chromatography-Mass Spectrometry

  • Yoon, Ok-Kyung;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.35-42
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    • 2009
  • Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

Measurement of Aldehydes in Replacement Liquids of Electronic Cigarettes by Headspace Gas Chromatography-mass Spectrometry

  • Lim, Hyun-Hee;Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2691-2696
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    • 2013
  • The electronic cigarette (E-cigarette) is a battery-powered device that aerosolizes nicotine so that it is readily delivered into the respiratory tract. The analytical data regarding the substances present in E-cigarettes are very limited. The aim of this study was to measure the concentration of aldehydes-formaldehyde (FA), acetaldehyde (AA) and, acrolein (AL)-in 225 replacement liquid brands from 17 E-cigarette shops sold in the Republic of Korea by headspace solid-phase micro extraction and gas chromatography-mass spectrometry (HS-SPME GC-MS). The concentration range of FA and AA was 0.02-10.09 mg/L (mean = 2.16 mg/L, detected in 207 of 225 samples) and 0.10-15.63 mg/L (mean = 4.98 mg/L, detected in all samples), respectively. AL was not detected in any of 225 replacement liquids. FA and AA were originally present in almost all replacement liquids of electronic cigarettes.