• Title/Summary/Keyword: Gas Chromatography(GC)

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Establishment of Pre-Harvest Residue Limit for Buprofezin and Penthiopyrad during Cultivation of Oriental melon (Cucumis melon var. makuwa) (참외(Cucumis melon var. makuwa)에 대한 Buprofezin 및 Penthiopyrad의 생산단계 잔류허용기준 설정)

  • Kim, Hea Na;Kim, Seong Beom;Choi, Eun;Woo, Min Ji;Kim, Ji Yoon;Saravanan, Manoharan;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.123-129
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    • 2014
  • The present work was aimed to determine the pre-harvest residue limits (PHRLs) and the safety management of commonly used pesticides namely buprofezin and penthiopyrad on oriental melon (Cucumis melon var. makuwa). In this study, the buprofezin (diluted two thousand fold) and penthiopyrad (diluted four thousand fold) were sprayed single time on oriental melon in the cultivation areas Sangju (site 1) and Sungju (site 2). Oriental melon were randomly collected from the both areas at the end of 0 (2 hours after pesticides spaying), 1, 2, 3, 5, 7, 9 and 10 days. For analysis, each samples were partitioned twice (80 and 70 mL) with dichloromethane and purified by florisil SPE cartridge. Finally, the residual amounts of both pesticides in all samples were analyzed using gas chromatography/nitrogen phosphorus detector (GC/NPD). In this study, the method limit of quantification (MLOQ) for both buprofezin and penthiopyrad in oriental melon was found to be $0.01mg\;kg^{-1}$ and their recovery levels were 91.1~98.6% and 90.0~104.6%, respectively. Further, the calculated biological half-life for buprofezin and penthiopyrad in oriental melon were 3.9 and 3.5, and 3.0 and 2.7 days in site 1 and 2, respectively. The results of this study found that the PHRLs for buprofezin and penthiopyrad were 4.24 and $2.31mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggest that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when oriental melon is harvested.

Monitoring of Residual Pesticides and Exposure Assessment of Olive Oil Products Sold on the Market (올리브유의 잔류농약 모니터링 및 노출량 조사)

  • Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.4
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    • pp.211-216
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    • 2023
  • A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

Translocation of Tolclofos-methyl from Ginseng Cultivated Soil to Ginseng (Panax ginseng C. A. Meyer) and Residue Analysis of Various Pesticides in Ginseng and Soil (토양 중 잔류된 Tolclofos-methyl의 인삼(Panax ginseng C. A. Meyer)에 대한 이행 및 잔류 특성)

  • Kim, Ji Yoon;Kim, Hea Na;Saravanan, Manoharan;Heo, Seong Jin;Jeong, Haet Nim;Kim, Jang Eok;Kim, Kwan Rae;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.130-140
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    • 2014
  • Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

Study of Trans Fatty Acids and Saturated Fatty Acids in Child-favored Foods (어린이 기호식품 중 트랜스지방 및 포화지방 실태조사)

  • Yoon, Tae-Hyung;Lee, Sung-Min;Shin, Hee-Jun;Lee, Soo-Yeon;Hong, Jin;No, Ki-Mi;Park, Kyoung-Sik;Leem, Dong-Gil;Lee, Kwang-Ho;Jeong, Ja-Young
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.40 no.11
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    • pp.1562-1568
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    • 2011
  • We studied the amounts of trans fatty acids and saturated fatty acids in child-favored foods. Confectioneries, breads, donuts and hamburgers were included in this study. The total fatty acid content and the amount of each type of fatty acid were determined by gas chromatography with a flame-ionized detector. Confectioneries were shown to have the highest content of crude fat. The mean content was 24.2${\pm}$6.9 (range: 4.6~41.1) g/100 g food. The mean content of crude fat in donuts, bread and hamburgers was 23.9${\pm}$5.8 (range: 14.1~39.5) g/100 g food, 15.7${\pm}$7.9 (range: 1.4~30.0) g/100 g food, and 9.5${\pm}$3.4 (range: 4.5~18.5) g/100 g food, respectively. Bread had the most trans fatty acids at 1.3 g/100 g food. This result inferred that manufacturers have tried to reduce the trans fat content. The mean content of saturated fatty acids in confectioneries, donuts, bread, and hamburgers was 11.6${\pm}$4.8 (range: 2.0~22.7) g/100 g food, 11.2${\pm}$4.0 (range: 4.8~23.2) g/100 g food, 6.9${\pm}$4.1 (range: 0.6~15.4) g/100 g food, 3.0${\pm}$1.0 (range: 1.0~5.8) g/100 g food, respectively. This content depended on crude fat. The composition of fatty acids varied according to the oil and fat used in the manufacturing process of each food, and the natural content. Foods that were fried in vegetable oil tended to be especially low in saturated fat.

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.

Evaluation of Butyltin Compounds and its Distribution Among Seawater, Sediment and Biota from the Kwangyang Bay (광양만내 유기주석화합물의 해수, 퇴적물, 생물중 농도 및 분포 상관관계)

  • KIM Gue Yoong;PARK Mi-Ok
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.34 no.4
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    • pp.291-298
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    • 2001
  • Seawater, sediment and biota in the Kwangyang Bay were analyzed by gas chromatography/quartz furnace atomic absorption spectroscopy (GC-QFAAS) to investigate concentrations and distribution pattern of butyltin compounds (TBT, DBT, MBT) during February, April and July, 1996, Marine biota analyzed were Tapes japcnicus and Crassostrea gigas. The concentrations of tributyltin (TBT) in seawater were in the range of ND-15.7 ng/L for the surface and ND-68.5 ng/L for the bottom. The highest concentration of TBT in seawater was detected in April for the both, surface and bottom water. The maximum value of $TBT_{(bottom)}/TBT_{(surface)}$, 3.6 in April showed the increased input of TBT from the surface water in April compared to February (2.1) and July (0.9). The concentrations of TBT in the sediment were in the range of ND-8.5 ng/g dry wt. The highest concentration of TBT in the sediment was measured in July, This result seems to attributed to the removal of TBT from water column via sorption onto particulate matters to the relatively undisturbed underlying sediment and increased input of TBT by increased fluxes of detritus of marine plankton after spring bloom, in July. The mean values of partitioning coefficient ($K_d$) of TBT between seawater and sediment were $3.0\times10^3$(February), $7.4\times10^3$(April) and $9.4\times10^3$(July). The concentrations of TBT in biosamples were in the range of ND-93.30 ng/g dru wt. (T. japonicus) and ND-138.53 ng/g dry wt. (C. gigas). The seasonal variation of TBT contents in biota was remarkable. The $K_d$ (biological concentration factor) was $7-41\times10^3$ for T. japonicus. and $5-34\times10^3$ for C. gigas. The measured TBT concentrations in seawater in the study area was sufficient to cause the imposex of shellfish and to retard the growth of aquatic organisms including oyster upon chronic exposure.

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Correlation between Steroid Hormone Metabolites and Leiomyomas of Uterus (자궁근종과 성호르몬 대사물과의 연관성)

  • Bai, Sang-Wook;Jung, Byung-Hwa;Chung, Bong-Chul;Jeon, Jin-Dong;Lee, Hyun-Jung;Kwon, Han-Sung;Chung, Kyung-Ah;Kim, Sei-Kwang;Park, Ki-Hyun
    • Clinical and Experimental Reproductive Medicine
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    • v.28 no.4
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    • pp.279-286
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    • 2001
  • Objective: To elucidate 1) whether there are any differences in the urine concentrations of steroid hormone metabolites between patients with leiomyoma and normal controls 2) the correlation between urinary profiles of steroid hormones and leiomyomas of the uterus according to their type, location, volume, and weight. Materials of Methods : The study population consisted of 37 premenopausal patients with uterine leiomyoma and the control group consisted of 25 premenopausal normal volunteer women without uterine leiomyoma. Confirmation of the existence of uterine leiomyoma was done by ultrasonography and histopathological examination after surgery. The volume of the leiomyoma was estimated by trans-abdominal and/or trans-vaginal ultrasonography. The Leiomyomas were divided into 3 types (subserosal, intramural and submucosal). Seventeen patients had subserosal type of leiomyoma, 10 with the intramural type and 10 with the submucosal type. The locations of the leiomyoma were also divided into 3 groups (fundus, body and isthmus). Seventeen patients showed a fundus location, 10 in body, and 10 in isthmus. We compared urinary profiles of the endogenous steroids between patients with leiomyomas and normal controls, and also investigated the relationship between urinary profiles of the endogenous steroids and leiomyomas according to their type, location, volume and weight by using highly sensitive Gas Chromatography-Mass Spectrometry (GC-MS) system. Results: The mean ages of the patients with leiomyomas and the control group were $43.1{\pm}5.6$ and $40.6{\pm}7.2$ years, the weights were $63.4{\pm}7.3$ and $59.4{\pm}8.1\;kg$, and their heights were $155.4{\pm}4.8$ and $159.3{\pm}4.8\;cm$ respectively. Seventeen patients had subserosal, 10 had intramural, and 10 had submucosal leiomyomas. There were 17 patients with leiomyoma located in fundus, 10 in body and 10 in isthmus. $17{\beta}$-estradiol, 5-AT, 11-keto ET, $11{\beta}$-hydroxy An, $11{\beta}$-hydroxy Et, THS, THA, THE, a-cortolone, a-cortol, $\beta$-cortol, $11{\beta}$-OH Et/$11{\beta}$-OH An and E2/E1 were significantly increased in patients with leiomyoma than in the control group. $17{\beta}$-estradiol was significantly increased in the intramural and the submucosal types than in the subserosal type. There was no significant difference in the concentrations of urinary steroids according to the locations of leiomyomas. There was no significant relationship between the concentration of urinary steroids and the volume of the leiomyomas. $17{\beta}$-estradiol significantly decreased as the weight of uterus increased (r=-0.322, p=0.04). Conclusion: The concentrations of steroid hormone metabolites were generally increased in patients with leiomyoma but were not significantly related to the volume and weight of the leiomyomas. Our study suggests that steroid hormones may be involved in the initiation of leiomyomas but may not be involved in their progression. In addition, the concentrations of steroid hormone metabolites are not related to the leiomyoma type and location.

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Case Study on Determination of the Level of New RoHS II Substances in Domestic Electronic and Electrical Equipments (국내 전기전자 제품에 함유된 신규 RoHS II 물질 검출 사례 연구)

  • Song, Moon-Hwan;Son, Seung-Hwan;Cho, Young-Dal;Choe, Eun-Kyung
    • Clean Technology
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    • v.17 no.2
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    • pp.124-133
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    • 2011
  • In addition to six substances regulated in EU RoHS including lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE), priority substances are identified in new RoHS II as hexabromocyclododecane (HBCDD), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP) and diethylhexyl phthalate (DEHP). In this study, 20 plastic samples were collected from 12 domestic electrotechnical companies and levels of four restricted substances were determined by gas chromatography-mass spectrometry, Among 20 parts that compose washer, refrigerator or microwave oven, HBCDD was detected in three samples of NBR material with the amount of 42~381 mg/kg while DBP and BBP was not detected in any samples collected respectively, implying that these substance may not be used widely in plastic materials for EEE. However, DEHP was detected in all samples of NBR, PP, PBT, EPDM and PVC materials with the amount of 42 up to 59,400 mg/kg that exceeds the limit value of 0.1 wt% (1,000 mg/kg). Presence of a restricted substance in polymer material makes a great negative influence on a number of final product. To cope with coming RoHS II as well as REACH, action not to use DEHP in plastic material or the relevant notification in case of REACH seems to be needed. Screening test of Arsenic compounds such as diarsenic pentaoxide, diarsenic trioxide, lead hydrogen arsenate, triethyl arsenate that are included in REACH SVHC was done by ICP measurement Arsenium was detected in four samples made of NBR and PBT materials in the level of 15~700 mg/kg. By considering the screening method used in this study, the amount of arsenium compounds in the thermistor made of PBT material has a high chance of exceeding the regulated limit value.

Evaluation of Odors and Odorous Compounds from Liquid Animal Manure Treated with Different Methods and Their Application to Soils (액상 가축분뇨의 처리 및 토양환원에 따른 악취 및 악취물질의 평가)

  • 고한종;최홍림;김기연;이용기;김치년
    • Journal of Animal Science and Technology
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    • v.48 no.3
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    • pp.453-466
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    • 2006
  • To comply with stricter regulations provoked by increasing odor nuisance, it is imperative to practice effective odor control for sustainable livestock production. This study was conducted to assess odor and odorous compounds emitted from liquid animal manure with different treatment methods such as Fresh Manure(without treatment, FM), Anaerobic Digestion(AD) and Thermophilic Aerobic Digestion(TAD) and their application to soil. Air samples were collected at the headspace of liquid manure, upland and paddy soil, and analyzed for odor intensity and offensiveness using an olfactometry; odor concentration index using odor analyser; nitrogen-containing compound such as ammonia(NH3) using fluorescence method; and sulfur containing compounds such as hydrogen sulfide(H2S), methyl mercaptan(MeSH), dimethyl sulfide(DMS) and dimethyl disulfide(DMDS) using gas chromatography-pulsed flame photometric detector, respectively. Odor intensity, offensiveness and concentration index from TAD liquid manure was statistically lower than those from FM and AD(p<0.01). Mean concentrations of H2S, MeSH, DMS, DMDS and NH3 were 65.93ppb, 18.55ppb, 5.26ppb, 0.33ppb and 10.57ppm for liquid manure with AD; and 5.15ppb, 0.97ppb, 0.80ppb, 0.56ppb and 1.34ppm for liquid manure with TAD, respectively. More than 60% of malodorous compounds related to nitrogen and sulfur were removed by heterotrophic microorganisms during TAD treatment. When liquid manure was applied onto upland and paddy soil, NH3 removal efficiencies ranged from 51 to 94% and 22 to 91% for AD and TAD liquid manure, respectively. The above results show that liquid manure with TAD is superior to AD and FM with respect to the odor reduction and odor problem caused by land applied liquid manure is directly related to the degree of odor generated by the manure treatment method.

Surfactant Enhanced In-Situ Soil Flushing Pilot Test for the Soil and Groundwater Remediation in an Oil Contaminated Site (계면활성제 원위치 토양 세정법을 이용한 유류 오염 지역 토양.지하수 정화 실증 시험)

  • 이민희;정상용;최상일;강동환;김민철
    • Journal of Soil and Groundwater Environment
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    • v.7 no.4
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    • pp.77-86
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    • 2002
  • Surfactant enhanced in-situ soil flushing was performed to remediate the soil and groundwater at an oil contaminated site, where had been used as a military vehicle repair area for 40 years. A section from the contaminated site (4.5 m $\times$ 4.5 m $\times$ 6.0 m) was selected for the research, which was composed of heterogeneous sandy and silt-sandy soils with average $K_d$ of 2.0$\times$$10^{-4}$cm/sec. Two percent of sorbitan monooleate (POE 20) and 0.07% of iso-prophyl alcohol were mixed for the surfactant solution and 3 pore volumes of surfactant solution were injected to remove oil from the contaminated section. Four injection wells and two extraction wells were built in the section to flush surfactant solution. Water samples taken from extraction wells and the storage tank were analyzed on a gas-chromatography (GC) for TPH concentration in the effluent with different time. Five pore volumes of solution were extracted while TPH concentration in soil and groundwater at the section were below the Waste Water Discharge Limit (WWDL). The effluent TPH concentration from wells with only water flushing was below 10 ppm. However, the effluent concentration using surfactant solution flushing increased to 1751 ppm, which was more than 170 times compared with the concentration with only water flushing. Total 18.5 kg of oil (TPH) was removed from the soil and groundwater at the section. The concentration of heavy metals in the effluent solution also increased with the increase of TPH concentration, suggesting that the surfactant enhanced in-situ flushing be available to remove not only oil but heavy metals from contaminated sites. The removal efficiency of surfactant enhanced in-situ flushing was investigated at the real contaminated site in Korea. Results suggest that in-situ soil flushing could be a successful process to remediate contaminated sites distributed in Korea.