• Title/Summary/Keyword: purge and trap method

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Optimum Extraction Methods of Volatile Compounds in Beef Extract Powder (쇠고기 엑기스 분말 휘발성 성분의 최적 추출방법에 관한 연구)

  • Kim Hun;Cho Woo-Jin;Jeong Eun-Jeong;Ahn Jun-Suck;Lim Chi-Won;Yoo Young-Jae;Kim Kwang-Ho;Cha Yong-Jun
    • The Korean Journal of Food And Nutrition
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    • v.17 no.4
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    • pp.412-419
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    • 2004
  • In odor to select optimum extraction methods of volatile compounds in beef extract powder(BEP) as basic data for the development of a new detection method of irradiated BEP, four extraction methods, such as solid phase microextraction with polar fiber(S-PD) and non-polar fiber(S-CD), purge and trap(P&T) and liquid liquid continuous extraction(LLCE) methods, were tested with gas chromatography/mass spectrometry method. A total of 106 volatile compounds including 22 hydrocarbons, 7 aldehydes, 6 ketones, 13 alcohols, 6 sulfur-containing compounds, 19 nitrogen-containing compounds, 6 aromatic compounds, 17 terpenes, 8 furans and 2 miscellaneous compounds were detected in BEP by four detection methods. The most compounds(62 compounds) were detected by S-PD method, followed by P&T(43), LLCE(38) and S-CD method(30). Among these methods, S-PD and P&T methods showed a complementary interrelationship to detect volatile compounds as S-PD method showed high detectabiltiy to all compound groups except hydrocarbons and ketones, which had high volatility and low molecular weight(less than RI 1200), but P&T method showed the contrary pattern to that of S-PD method. Moreover, the most of volatile compounds detected by S-CD and LLCE methods were also detectable by S-PD or/and P&T methods. Therefore, the simultaneous application of S-PD and P&T methods were selected as the optimum volatile extraction methods of BEP.

Analysis of mercury and methylmercury in river sediment samples (하천퇴적물 중의 수은 및 메틸수은 분석 연구)

  • Lee, Jung-Sub;Park, Jae-Sung;Kang, Hak-Gu;Cho, Jae-Seok;Hong, Eun-Jin;Jeong, Gi-Taeg;Cha, Jun-Seok;Jung, Kwang-Yong;Kim, Young-Hee
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.44-50
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    • 2009
  • In this study, the use of purge & trap GC-MS technique for determination of methylmercury in sediment samples was described. The method detection limit of the method was determined as 0.06 ng/g and the recovery of the method was $102{\pm}11.4%$, with precisions better than 11.2%. The method was validated by analysis of CRMs such as ERM CC580 (estuarine sediment) and IAEA 405 (sediment). Additionally, the performance of the method was tested on river sediment samples and the analytical results were compared with those of the GC-CVAFS, which has been widely used for methylmercury analysis.

Analysis of 1,4-Dioxane and Chlorohydrins in Food Additives by Purge & Trap GC (퍼지앤트랩-기체크로마토그래피(PT-GC)를 이용한 식품첨가물 중 1,4-디옥산 및 클로로히드린류 분석)

  • 조태용;신영민;반경녀;오세동;이창희;이영자;문병우
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.32 no.7
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    • pp.965-970
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    • 2003
  • This study has been performed to develope a method for the simultaneous determination of 1,4-dioxane (DOX), epichlorohydrin (EPC), propylene chlorohydrin (PCH), ethylene chlorohydrin (ECH) and 1,3-dichloro-2-pro-panol (DCP) in polysorbates, chloline chloride, choline bitartrate, modified starch and spices by purge and trapgas chromatography. Experimental design was used to select a suitable trap by measuring the limit of detection (LOD) and to investigate the effect of temperature and salt of extraction, and the percentage of recovery in various matrix. The LOD of DOX, EPC, PCH, ECH and DCP were 1.38$\mu\textrm{g}$, 0.23$\mu\textrm{g}$, 3.30$\mu\textrm{g}$, 3.97$\mu\textrm{g}$, 20.43$\mu\textrm{g}$ respectively, by means of using Vorcarb 3000 trap with 5$0^{\circ}C$ sample sparger. Excluding EPC, the recoveries of target compounds were above 90% in all matrix. Target compounds in polysorbates (17), choline chloride (5), choline bitartrate (5), modified starch (8) and spices (25) were not detected. But 2.5 ppm of DOX was detected in Tween 80.

Changes of Volatile Flavor Compounds in Traditional Kochujang during Fermentation (재래식고추장 숙성과정 중의 휘발성 향기성분의 특성)

  • Choi, Jin-Young;Lee, Taik-Soo;Park, Sung-Oh;Noh, Bong-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.4
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    • pp.745-751
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    • 1997
  • Volatile flavor components of kochujang made from a glutinuous rice by traditional method were analyzed by using purge and trap method during fermentation, and identified with GC-MSD. Fifty-one volatile components including 19 alcohols, 13 esters, 7 acids, 3 aldehydes, 1 alkanes, 2 ketones, 2 amines, 1 benzene, 1 alkene, 1 phenol and others were found in kochujang made by traditional method. The number of volatile components detected immediately after making kochujang were 22 and increased to 41 components after 30 day of fermentation. The most number 51 of volatile components were found after 120 day of fermentation. Twenty-two volatile components were commonly found through the fermentation period such as acetic acid ethyl ester, ethanol, butanoic acid ethyl ester, 1-butanol, 2-methyl-1-propanol, 3-methyl-1-butanol, butanoic acid and ethenone. Peak area(%) of 1-butanol was the highest one among the volatile components at immediately after mashing while ethanol showed the highest peak area after 30 day of fermentation. Although the various types of peak areas of volatile components were shown in kochujang during the fermentation days, acetic acid-ethyl ester, ethanol, butanoic acid-ethyl ester, 1-butanol, 3-methyl-1-butanol and 2-methyl-1-propanol were mainly detected during fermentation. Those might be the major volatile components in kochujang made by traditional method.

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Volatile Flavor Components in Pumpking Vinegar

  • Hur, Sung-Ho;Lee, Wonkoo
    • Preventive Nutrition and Food Science
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    • v.3 no.2
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    • pp.119-122
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    • 1998
  • Pumpkin venegar was produced using autoclaved pumpkin juice by fermenting with cetobacter starter and ethanol at the ratio of 4 % and 10% to the volume of pumpkin juice, respectivley. Fermentation was carried out at 2$0^{\circ}C$ for 14 days followed by aging at 1$0^{\circ}C$ for 14 days. Flavor components of pumpkin vinegar was determined using GC/MS. Identified components, were 2 aldehydes (4.74%), 5 acohols (30.06%), 4 ketones (8.99%), 4 acids (16.39%), 5 alkanes (11.10%), 11 miscellaneous compounds (27.01%) and 9 unknown compounds (1.71%). Pumpkin vinegar showed very similar flavor characteristics to those of conventional wien vinegar and sherry wine vinegar in particular , acetioin, methyl acetate, and butanoic acid were typical volatile components of these three kinds of vinegar. Pumpkin vinegar showed possiblity to compete with European wine vinegar.

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Chracteristics of volatile flavor compounds in improved kochujang prepared with soybean koji during fermentation (콩고오지를 사용한 개량식고추장의 숙성과정 중 휘발성 향기성분의 특성)

  • Choi, Jin-Young;Lee, Taik-Soo;Park, Sung-Oh
    • Korean Journal of Food Science and Technology
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    • v.29 no.6
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    • pp.1144-1150
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    • 1997
  • Volatile flavor components of soybean koji kochujang made from a glutinuous rice by improved method were analyzed by using a purge and trap method during fermentation, and identified with GC-MSD. Fifty-six volatile flavor components including 16 alcohols, 15 esters, 7 acids, 4 aldehydes, 5 alkanes, 3 ketones, 1 benzene, 1 alkene, 2 phenol and 2 others were found in improved kochujang. The number of volatile flavor components detected immediately after making kochujang were 32 and increased to 46 components after 30 day of fermentation. The most number 55 of volatile flavor components were found after 90 day of fermentation. Thirty-one kinds of volatile flavor components were commonly found through the fermentation period 9 alcohols such as 2-methyl-1-propanol, ethanol, 3-methyl-1-butanol, 8 esters such as methyl acetate, ethyl acetate, 2-methylpropyl acetate, 3 aldehydes such as butanal, acetaldehyde, furfural and 11 othesrs. Although the various types of peak areas (%) of volatile flavor components were shown in kochujang during the fermentation days, ethanol. ethyl acetate, ethyl butanoate, 2-methylpropyl acetate, 2-methyl-1-propanol and 3-methyl-1-butanol were mainly detected during fermentation. Those might be the major volatile flavor components in kochujang made by improved method. Peak area of ethanol was the highest one among the volatile flavor components at immediately after mashing and 90 day while ethyl acetate showed the highest Peak area after $30{\sim}60$ day of fermentation and 3-methyl-1-butanol showed the highest peak area after $120{\sim}150$ day of fermentation.

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Studies on the Quantitative analysis and the Health Effect of VOCs in Environment - Analysis for THMs of tap water in six cities of Korea - (VOCs 측정 및 VOCs가 인체에 미치는 영향에 관한 연구 - 우리나라 6개 대도시 수도수 중 THMs 분석 -)

  • Kim, Mi-Kyoung;Park, Yuon-Sin;Chung, Yong
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.55-65
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    • 2000
  • In this study, we collected the tap water that treated from water plant in Seoul, Incheon, Taejon, Kwangju, Taeku and Pusan and supplied each house. The sampling period was June and September, 1997. The concentration of THMs formed by chlorination in drinking water was determined with the purge and trap method with GC/MSD recommended by the us EPA 542.2 method. Chloroform is the most of THMs (47.43%~93.11%) and the content order is bromodichloromethane > chlorodibromomethane > bromoform. In Incheon, Taejon, Kwangju, Taeku and Pusan, the content of bromodichloromethane, chlorodibromomethane and bromoform was higher than Seoul. But, in June and September, the concentration of THMs in six cities is not over Korea Drinking Water Regulation $100{\mu}g/L$. The calculated human exposure for each substances were chloroform $6.14{\times}10^{-4}mg/kg/day$, bromodichloromethane $1.01{\times}10^{-4}mg/kg/day$, chlorodibromomethane $0.29{\times}10^{-4}mg/kg/day$, bromoform $0.01{\times}10^{-4}mg/kg/day$ and THMs $7.98{\times}10^{-4}mg/kg/day$.

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A Simple and Simultaneous Analysis of Volatile Halogenated Hydrocarbons in Indoor Air Using Personal Sampler

  • Jung, Won-Tae;Sohn, Dong-Hun
    • Journal of Korean Society for Atmospheric Environment
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    • v.9 no.E
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    • pp.373-381
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    • 1993
  • To understand the human exposure levels of volatile halogenated hydrocar-bons in ambient air, a new rapid and convenient analytical method for determination of the compounds in gaseous phase was evaluated and established. The method is based upon passsive diffusion to personal sampler containing adsorbent and solvent extraction followed by purge trap/ on-column cryof-ocusing method. A new method needs no special instrumentation for gas collection because it is based upon the passive diffusion principle. The typical chromatogram obtained in this study proved that rapid and simultaneous determination of target analytes was possible with good resolution. The developed method was successfully applied to determine the volatile halogenated hydrocarbons in indoor air and the values obtained by this new method were compared with those by direct suction method. The concentration of carbon tetrachloride, 1,1,2-trichloroethylene, chloroform showed the values below 400$\mug/m^3$ except the maximum of 1,513$\mug/m^3$ of chloroform. 1,1,1-Trichloroethane showed approximately 1,000 to 5,000$\mug/m^3$ range of diurnal fluctuation in indoor air.

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A Study on the Development of Analytical Method for Micro-Odorous Compounds in Water (흡착제를 이용한 수중의 미량 이취물질 분석법 개발에 관한 연구)

  • 김은호;성낙창;최용락
    • Journal of Life Science
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    • v.9 no.5
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    • pp.575-580
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    • 1999
  • Even if odorous compounds remained very low concentration in water, it caused strong odor. Because Geosmin and most of odorous compound had very vaporization, those were difficult to analyze with GC/MSD and Purge & Trap. So, we needed pre-treatment method for decreasing amounts of extracting solvents, improving recovery efficiencies and increasing analytical efficiencies. This study developed efficient technology for analyzing odorous compounds, using various adsorbents and extracting solvents. The optimum adsorbent was XAD resins. Especially, XAD-2, XAD-7 and XAD-2010 were superior, but XAD-2 of these and MTBE was the optimum extraction solvent. Other extraction solvent's efficiency was in order of MTBE>Dichloromethane>n-Hexane>Diethylether. The optimum NaCl dosage for increasing efficiency was 5g in liquid-liquid extraction method. The shaking time(0∼24hr) had no concern with adsorption efficiency. The optimum adsorbent was XAD-2 resin and extraction solvent was MTBE. Dosing NaCl, adsorption efficiency was increased in liquid-liquid extraction method, but NaCl has no effect on liquid-solid extraction method. In this experimental results, this method will apply to not only Geosmin but other well-known odorous compounds (2-MIB, IBMP, IPMP, TCA) and algae toxins (Mycrocystin, Anatoxin etc)

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A Study on the Development of Analytical Method for Micro-odorous Compounds in Water (흡착제를 이용한 수중의 미량 이취물질 분석법 개발에 관한 연구)

  • Kim, Eun-Ho;Son, Hee-Jong;Kim, Yeong-Ung;Kim, Hyeong-Seok;Sung, Nak-Chang
    • Journal of Environmental Health Sciences
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    • v.25 no.3
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    • pp.103-107
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    • 1999
  • Even if odorous compounds remain very low concentration in water, it cause strong odor. Because Geosmin and most of odorous compound had very low vaporization, those were difficult to analyze with GC/MSD and Purge & Trap. So, we needed pre-treatment method for decreasing amounts of extracting solvents, improving recovery efficiencies and increasing analytical efficiencies. This study developed efficient technology for analyzing odorous compounds, using various adsorbents and extracting solvents. The optimum adsorbent was XAD resins. Especially, XAD-2, XAD-7 and XAD-2010 were superior, but XAD-2 of these and the optimum extraction solvent is MTBE. Other extraction solvents' efficiency is in order of MTBE>Dichloromethane>n-Hexane>Diethylether. The optimum NaCl dosage for increasing efficiency is 5 g in liquid-liquid extraction method. The shaking time(0~24hr) has no concern with adsorption efficiency. The optimum adsorbent is XAD-2 resin and extraction solvent is MTBE. Dosing NaCl, adsorption efficiency is increased in liquid-liquid extraction method, but NaCl has no effect on liquid-solid extraction method. In this experimental results, this algae toxins(Mycrocystin, Anatoxin etc.).

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