• Title/Summary/Keyword: Solid-phase microextraction

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Analysis of Odorous compounds in Air by Solid Phase Microextraction (SPME) (SPME 분석법을 이용한 대기중 악취물질의 분석)

  • 허귀석;김대원
    • Proceedings of the Korea Air Pollution Research Association Conference
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    • 2001.11a
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    • pp.340-341
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    • 2001
  • 대기중의 악취물질의 분석은 현행 우리나라 악취공정시험법에 고시되어 있으나 복잡한 농축장치를 필요로하고 조작법이 복잡하고 시간이 많이 소요된다. 주요 악취물질로서 암모니아, 메틸머캅탄, 황화수소, 이황화메틸, 아세트알데히드등은 극미량에서(pub) 악취를 발생시키는 악취 주요물질이다. 그러나 이 물질들은 흡착, 반응성이 커서 정확한 분석이 어렵다. 본 연구에서는 간단한 장치로서 시료농축이 가능하며, 간단히 GC injection에 주입, 분석할 수 있는 SPME법을 이용하여 악취물질을 신속하게 분석할 수 있는 분석법을 개발하고저 하였다. 분석방법에 대한 분석재현성, 분석한계를 조사하였으며, 이 분석방법이 앞으로 악취물질분석방법으로 활용될 수 있도록 기본 분석법을 확립하고자 하였다. (중략)

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Effects of Staphylococcus carnosus on Quality Characteristics of Sucuk (Turkish Dry-Fermented Sausage) During Ripening

  • Kaban, Guzin;Kaya, Mukerrem
    • Food Science and Biotechnology
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    • v.18 no.1
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    • pp.150-156
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    • 2009
  • In this study, Staphylococcus carnosus isolated from traditional sucuk (Turkish dry-fermented sausage) was used in combination with Lactobacillus plantarum as a lactic culture in sucuk production. Sucuk produced with only L. plantarum was evaluated as a control group. Microbiological, physicochemical, and volatile profile characteristics of sucuk samples were investigated during ripening. In both sausages with S. carnosus and control group, pH value decreased to below 5.0 at the $3^{rd}$ day. In all samples, Aw value decreased as the ripening time progressed. Sausages with S. carnosus showed the higher nonprotein nitrogen (NPN) value than control group. However, the highest mean value for thiobarbituric acid reactive substances (TBARS) was observed in control group. Enterobacteriaceae dropped to undetectable levels at the $3^{rd}$ day in both groups. S. carnosus increased approximately 1 log unit within the first 3 days of the fermentation. In the presence of S. carnosus, significant changes were observed in only a few volatile compounds.

Volatiles from the Maillard Reaction of L-Ascorbic Acid and L-Alanine at Different pHs

  • Yu, Ai-Nong;Deng, Qi-Hui
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1495-1499
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    • 2009
  • The volatiles formed from the reactions of L-ascorbic acid with L-alanine at 5 different pH (5, 6, 7, 8, or 9) and $140{\pm}2^{\circ}C$ for 2 hr was performed using solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) analysis were identified to be 25 different kinds. The reaction between L-ascorbic acid and L-alanine led mainly to the formation of pyrazines. Many of these were alkylpyrazines, such as 3-ethyl-2,5-dimethylpyrazine, 2,5-dimethylpyrazine, 2-ethyl-5-methylpyrazine, 3,5-diethyl-2-methylpyrazine, methylpyrazine, 2-ethyl-6-methylpyrazine, and 2,3-diethyl-5-methylpyrazine, other compounds identified were furans, phenols, benzoquinones, 2,4,6-trimethylpyridine, and 2-methylbenzoxazole. The studies showed that furans, such as furfural and benzofuran were formed mainly at acidic pH. In contrast, higher pH values could promote the production of pyrazines.

Optimization of Headspace Analysis of Volatile Compounds from Oxidized Fish Oil

  • Shin, Eui-Cheol;Jang, Hae-Jin;Lee, Hyung-Il;An, Hae-Jung;Lee, Yang-Bong
    • Preventive Nutrition and Food Science
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    • v.8 no.4
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    • pp.315-320
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    • 2003
  • Headspace volatile compounds of oxidized fish oil were analyzed by the combination of hexane solvent or solid phase microextraction, gas chromatography and mass selective detector. The optimum condition of headspace analysis by hexane trapping was 23 min absorption time, 96$^{\circ}C$ sample temperature and 20 mL/min air flow rate. The numbers of volatile compounds identified by solvent trapping and SPME were 35 and 14, respectively. Groups having the largest amount and many kinds were hydrocarbons and aldehydes, respectively. The numbers of aldehydes were 15 and 6 for solvent trap and SPME, respectively. These basic data could be used as indicators for the quality changes of fish oil.

The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque (고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법)

  • Ahn Sang-Woo;Lee Si-Jin;Chang Soon-Woong
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.

Analysis of Breath from Diabetic Patients Based on a One-chip-type Sensor Array

  • Yu, Joon-Boo;Jang, Byoung Kuk;Byun, Hyung-Gi
    • Journal of Sensor Science and Technology
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    • v.28 no.4
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    • pp.221-224
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    • 2019
  • Based on the results of studies on acetone excretion in diabetic patients, a one - chip sensors array was fabricated by combining acetone-selective sensor materials and volatile-organic-compound sensitive sensor materials. An electonic-nose was implemented using a sensor array and confirmed selectivity for five gases. In this system, the excretion of diabetic patients and controls was sampled with solid phase microextraction fiber and transferred to the sensor array. Although the control and diabetic patients were distinct, several samples failed. In the control group, the results of blood tests were normal, but patients were highly obese. In addition, the gas chromatography mass spectrometry results for the subjects revealed chemicals that are external factors.

Flavor identification and analysis of fermented soybean pastes

  • Da-Na Lee;Kyung-Min Lee;Sung-Eun Lee;Tae-Oh Kim
    • Food Science and Preservation
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    • v.31 no.3
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    • pp.374-384
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    • 2024
  • Soybean paste is a staple food used to make doenjang (DE), cheonggukjang (CGJ), and miso (MI). In this study, solid-phase microextraction followed by gas chromatography-mass spectrometry was used to identify volatile components in DE, CGJ, and MI, and principal component analysis (PCA) was performed to determine their correlation between soybean pastes. Esters and hydrocarbons accounted for more than 55% of the total volatile components. PCA showed that esters were highly correlated with DE; pyrazines were correlated with CGJ; and alcohols were highly correlated with MI. Because DE, CGJ, and MI are made of the same material, their overall volatile content tended to be similar. However, the main volatile components and fragrances were different. These findings will be used as basic research data to promote quality improvement of soybean-based fermented foods in Korea and Japan.

Composition and Cell Cytotoxicity of Essential Oil from Caryopteris incana Miq. in Korea (층꽃나무(Caryopteris incana Miq) 정유의 성분 분석과 세포 독성 평가)

  • Kim, Song-Mun
    • Applied Biological Chemistry
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    • v.51 no.3
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    • pp.238-244
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    • 2008
  • The essential oil was obtained from the aerial part of Caryopteris incana Miq. by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GCMS). The fragrance of the essential oil was fougere and woody. There were sixty-nine constituents in the essential oil: 28 carbohydrates, 22 alcohols, 7 acetates, 7 ketones, 3 aldehydes, and 2 others. Major constituents were 4,6,6-trimethyl [1S-($1{\alpha},2{\beta},5{\alpha}$)]-bicyclo[3.1.1]hept-3-en-2-ol (11.8%), taucadinol (9.4%), myrtenyl acetate (9.2%), pinocarvone (7.0%), 1-hydroxy-1,7-dimethyl-4-isopropyl-2,7-cyclodecadiene (6.3%), ${\delta}$-3-carene (6.2%). By SPME extraction, forty-nine constituents were identified: 22 hydrocarbons, 16 alcohols, 6 acetates, 3 ketones, and 2 ethers. Major constituents of the SPME-extracted sample were ${\delta}$-3-carene (12.6%), (-)-myrtenyl acetate (11.2%), 6,6-dimethyl-2-methylene-bicycol [3.1.1] heptan-3-o1 (10.9%), pinocarvone (9.3%). By HS extraction, ten constituents were identified: 5 hydrocarbons, 2 amines, 1 alcohol, and 2 others. Major constituents of the HS-extracted sample were (Z)-2-fluoro-2-butene (34.9%), ${\delta}$-3-carene (6.9%), 6-(4-chlorophenul)tetrahydro-2-methyl-2H-1,2-oxazine (5.9%). The $IC_{50}$ value (0.011 ${\mu}g/mg$) in MTT assay using HaCaT keratinocyte cell line was lower than those of commercially-selling rosemary and tea tree, suggesting more toxicological studies are needed for commercial use of the essential oil of Caryopteris incana Miq.

Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Thermodynamic Studies on the Adsorption of 4-Octylphenol on Carboxen by GC/MS Analysis (GC/MS 분석에 의한 4-Octylphenol의 Carboxen 흡착에 대한 열역학적 연구)

  • Lee, Joon-Bae;Park, Woo-Yong;Shon, Shungkun;Jung, Ji Eun;Jeong, Yong Ae;Gong, Bokyoung;Kim, Yu-Na;Kwon, O-Seong;Paeng, Ki Jung
    • Applied Chemistry for Engineering
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    • v.29 no.3
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    • pp.356-361
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    • 2018
  • It is common to analyze volatile organic compound (VOC) or semi-VOC (SVOC) in a sample composed of a complex matrix consisting of multiple components such as bloods through a separation process. Adsorption is a physical phenomenon in which certain components accumulate on the surface of other phases. In order to overcome difficulties in the pretreatment process, an adsorption is frequently used. Solid phase microextraction (SPME) equipment with porous carbon carboxen (CAR) is an example of adsorption application. In this study, the adsorption of 4-octylphenol to carboxen was examined. To do so, the extraction efficiency for such solvents as dichloromethane ($CH_2Cl_2$, DCM), ethylacetate ($CH_3COOC_2H_5$, EA) and diethylether ($C_2H_5OC_2H_5$, $Et_2O$) was studied and also the derivatization reaction for 4-octylphenol with reagents of bistrimethylsilyltrifluoroacetamide (BSTFA), methylchloroformate (MCF) and pentafluorobenzylbromide (PFBBr) was compared. The combination of DCM and BSTFA showed good performance thus they were adopted for this study. Thermodynamic adsorption experiments showed that the adsorption process was endothermic and Freundlich isotherm equation was more suitable than Langmuir isotherm. It was also found that the adsorption followed a pseudo-$2^{nd}$ order kinetic model.