• Title/Summary/Keyword: GC-MS (SIM)

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Estimation of Estrogenic Activity by E-screen Assay and Stepwise Analysis of Endocrine Disruptors in Pilot Sewage Treatment Plant (파일럿 규모의 하수 처리 공정별 E-screen Assay에 의한 에스트로겐 활성과 내분비계 장애물질의 농도 평가)

  • Lee, Ji-Ho;Park, Jong-Yol;Ra, Jin-Sung;Duong, Cuong N.;Lee, Byoung-Cheun;Kim, Sang-Don
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.7
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    • pp.697-703
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    • 2006
  • Endocrine disruptors were measured with GC/MS in effluents discharged from sewage treatment processes in pilot scale for the purpose of water reuse. From that analysis, we compared the removal rate of them by treatment processes. Nonylphenol was mainly detected in effluents and high concentration from 0.36 to 0.94 ${\mu}g/L$. $17{\beta}$-estradiol(E2) and $17{\alpha}$-ethynylestradiol(EE2) were detected as below the limit of detection in effluent. Endocrine disruptors were removed effectively in the range from 50 to 100% by treatment process. EC50 value($9.0{\times}10^{-3}$ M) of $17{\beta}$-estradiol(E2) by dose response curve of E-screen assay has higher than that of bisphenol A($2.736{\times}10^{-5}M$) and p-octylphenol($9.760{\times}10^{-6}$ M). These results showed that alkylphenols have lower relative estrogen potency than other estrogens such as $17{\beta}$-estradiol(E2). Calculated estrogenic activity(ng-EEQ/L) was 2 times higher than measured total estrogenic activity which estimated by E-screen assay. Moreover estrogenic activity of effluent by treatment process showed very low as below 1 ng-EEQ/L.

Gibberellin A4 Producted by Fusarium solani Isolated from the Roots of Suaeda japonica Makino (칠면초의 뿌리로부터 분리된 Fusarium solani에 의해 생산된 지베렐린 A4)

  • Seo, Yeonggyo;You, Young-Hyun;Yoon, Hyeokjun;Kang, Sang-Mo;Kim, Hyun;Kim, Miae;Kim, Changmu;Lee, In-Jung;Kim, Jong-Guk
    • Journal of Life Science
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    • v.22 no.12
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    • pp.1718-1723
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    • 2012
  • Ten endophytic fungi with different colony morphologies were isolated from the roots of Suaeda japonica Makino growing naturally in Suncheon Bay. Plant growth promotion was verified by treating waito-c rice seedlings with culture filtrates from the endophytic fungi. The bioassays showed that the Sj/7/4 fungal strain induced effective growth promotion in the seedlings. The gibberellins (GA) produced by fungal strain Sj/7/4 were analyzed by gas chromatography /mass spectroscopy with selected ion monitoring (GC/MS SIM). The culture filtrate of Sj/7/4 fungal strain was confirmed to contain $GA_4$ through quantitative analysis. The Sj/7/4 fungal strain was identified to determine the internal transcribed spacer (ITS) regions with universal primers ITS-1 and ITS-4 by using polymerase chain reactions (PCR). Molecular analysis of the Sj/7/4 fungal strain showed high similarity to Fusarium solani. The Sj/7/4 fungal strain isolated from the root of S. japonica was therefore designated as F. solani Sj/7/4.

Studies on the Volatile Aroma Components of Pleurotus ostreatus (느타리버섯의 향기(香氣) 성분(成分)에 관한 연구(硏究))

  • Hong, Jai-Sik;Lee, Ji-Yul;Kim, Young-Hoi;Kim, Myung-Kon;Jung, Gi-Tae;Lee, Keug-Ro
    • The Korean Journal of Mycology
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    • v.14 no.1
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    • pp.31-36
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    • 1986
  • The volatile aroma concentrates were isolated from Pleurotus ostreatus by simultaneous distillation-extraction and analyzed by gas chromatography and combined gas chromatography-mass spectrometry. The aroma concentrates obtained had a typical raw or slightly cooked mushroom-like odor, and the yield was 123 ppm. Of 27 components identified, the major components were 3-octanone, 3-octanol, 2-octenal, n-octanol and 2, 4-decadienal, including 1-octen-3-ol contributing 67.06% of the total volatiles, and the $C_8$ compounds comprised about 80% of the total volatiles. On the other hand, the $C_6$ and $C_8$ alcohols in mushroom increased gradually with increase of standing time after homogenation, while aldehydes, ketones, and linoleic acid decreased, and also $C_6$ and $C_8$ compounds were significantly increased when linoleic and linolenic acid were added in homogenates. It appears that most of volatile aroma components in Pleurotus ostreatus were probably produced enzymatically from unsaturated fatty acids containing cis, cis-1, 4-pentadiene moiety.

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High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation (고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발)

  • Lee, Young-Deuk;Oh, Jae-Ho;Jang, Sang-Won
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.389-400
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    • 2011
  • A high-performance liquid chromatographic (HPLC) method was developed to determine residues of phenothrin and silafluofen, known as synthetic pyrethroids, in agricultural commodities. Insecticide residues were extracted with acetone from representative samples of four crops which comprised rice, apple, pepper and cabbage. The extract was purified serially by liquid-liquid partition and Florisil column chromatography. For rice and pepper samples, acetonitrile/n-hexane partition was additionally adopted to remove nonpolar interferences. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate two phenothrin isomers and silafluofen from sample co-extractives. Intact parent compounds were sensitively detected by ultraviolet absorption at 226 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine phenothrin and silafluofen residues at 0.02 and 0.01 mg/kg, respectively. Mean recoveries of phenothrin and silafluofen from four crop samples fortified at three levels in triplicate were in the range of 82.4~109.8% and 83.7~109.8%, respectively. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types and spiking levels. A selected-ion monitoring (SIM) LC/mass spectrometry (MS) with electrospray ionization was provided to confirm the suspected residue of phenothrin, even though no sufficient ionization of silafluofen was obtained. Both phenothrin and silafluofen could be successfully confirmed by gas chromatography/MS SIM with electron impact at 70 eV. The proposed method is sensitive, repeatable and rapid enough to apply to officially routine inspection of agricultural products.

Planting Conditions of Korean Cannabis Derived from Stable Isotope Ratio & Tetrahydrocannabinol Contents (안정동위원소 비율 및 테트라하이드로칸나비놀 함량 분석을 통한 한국산 대마의 재배 환경 추론)

  • Lee, Jae-Sin;Park, Yong-Hoon;Rhee, Jong-Sook;Jeong, Jin-Il;Lim, Mi-Ae;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.52 no.3
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    • pp.172-175
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    • 2008
  • Stable isotope ratio of carbon and nitrogen ($\delta^{13}C$ & $\delta^{15}N$), and $\Delta^{9}$-tetrahydrocannabinol (THC) contents were measured on 37 Korean cannabis and 10 commercial grade marijuana seized in Korea. Factors influencing on the measured values and their variations were investigated. $\delta^{13}C$ value of cannabis is specified mainly by water availability. Korean cannabis showed relatively low $\delta^{13}C$ values ranging -33.29$\sim$-27.01% (mean=-31.01%), which reflect geographic conditions of Korea where is rainy, especially during summer. $\delta^{15}N$ values, which reflect individual planting conditions, were relatively high up to -0.5$\sim$18.0% (mean=6.44%). It reflects characteristics of Korean cannabis growing wild in forest or cultivated in fertile soil. Tetrahydrocannabinol is the major hallucinogenic compound of cannabis. Ethanol extracts of cannabis leaves were derivatized by N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), and the derivatives were analyzed by GC-MS in selected ion monitoring (SIM) mode. THC contents of Korean cannabis ranged 0.11$\sim$4.34% (mean=1.47%), which were relatively low compared with commercial grade marijuana.

Identification of Petroselinic Acid (Cis-6-octadecenoic Acid) in the Seed Oils of Some of the Family Umbelliferae (Panax schinseng, Aralia continentalis and Acanthopanax sessiliflorus) by GC-MS, IR, $^1H-and$ $^13C-NMR$ Spectroscopic Techniques

  • Kim, Seong-Jin
    • Journal of the Korean Applied Science and Technology
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    • v.22 no.4
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    • pp.323-331
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    • 2005
  • Fatty acid compositions of the seed oils of P. schinseng, A. continentalis and A. sessiliflorus, were analyzed by gas chromatography (GC) equipped with a capillary column. A large unusual peak was observed just before the peak corresponding to oleic acid $(cis-9-C_{18:1})$. This unknown fatty acid was isolated by silver ion chromatography and then derivatized into the picolinyl ester. The mass spectrum of the picolinyl ester showed molecular ion at m/z=373 with other diagnostic ions such as m/z=178, 218, 232, 246, 274, 288, 302 and 344. Characteristic absorption peaks at $720\;cm^{-1}$, $1640\;cm^{-1}$ and $3010\;cm^{-1}$ in IR spectrum indicated the presence of cis-configurational double bond in the molecule. The $^1H-NMR$ spectrum of this acid gave two quintets centered at ${\delta}1.638$ (2H, C-3) and ${\delta}1.377$ (2H, C-4), and two multiplets centered at ${\delta}2.022{\sim}2.047$ (2H, C-5) and ${\delta}2.000{\sim}2.022$ (2H, C-8), and multiplet signals of olefinic protons centered at ${\delta}5.3015{\sim}5.3426$ (C-6, J=9.5 Hz) and ${\delta}\;5.3465{\sim}5.3877$ (C-7, J=9.5 Hz). The $^13C-NMR$ spectrum showed 18 carbon resonance signals including an overlapped signal at ${\delta}29.7002$ for C-12 and ${\delta}29.6520$ for C-13 (or they can be reversed), and other highly resolved signals at ${\delta}33.950$, ${\delta}24.558$, ${\delta}26.773$ and ${\delta}27.205$ due to C-2, C-3, C-5 and C-8 of a ${\Delta}^6-octadecenoic$ acid, respectively. From analysis results this unknown fatty acid could be identified as cis-6-octadecenoic acid. The seed oils of P. schinseng and A. sessiliflorus contained petroselinic acid (59.7%, 56.0%), oleic acid (18.3%, 6.1%) and linoleic acid (16.2%, 30.4%) with small amount of palmitic acid (3.0%, 3.1%) while the seed oil of A. continentalis comprised mainly oleic acid (30.2%), petroselinic acid (29.0%), linoleic acid (24.1%) and palmitic acid (13.1%).

Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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Brief Introduction of Research Progresses in Control and Biocontrol of Clubroot Disease in China

  • He, Yueqiu;Wu, Yixin;He, Pengfei;Li, Xinyu
    • 한국균학회소식:학술대회논문집
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    • 2015.05a
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    • pp.45-46
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    • 2015
  • Clubroot disease of crucifers has occurred since 1957. It has spread to the whole China, especially in the southwest and nourtheast where it causes 30-80% loss in some fields. The disease has being expanded in the recent years as seeds are imported and the floating seedling system practices. For its effective control, the Ministry of Agriculture of China set up a program in 2010 and a research team led by Dr. Yueqiu HE, Yunnan Agricultural University. The team includes 20 main reseachers of 11 universities and 5 institutions. After 5 years, the team has made a lot of progresses in disease occurrence regulation, resources collection, resistance identification and breeding, biological agent exploration, formulation, chemicals evaluation, and control strategy. About 1200 collections of local and commercial crucifers were identified in the field and by artificiall inoculation in the laboratories, 10 resistant cultivars were breeded including 7 Chinese cabbages and 3 cabbages. More than 800 antagostic strains were isolated including bacteria, stretomyces and fungi. Around 100 chemicals were evaluated in the field and greenhouse based on its control effect, among them, 6 showed high control effect, especially fluazinam and cyazofamid could control about 80% the disease. However, fluzinam has negative effect on soil microbes. Clubroot disease could not be controlled by bioagents and chemicals once when the pathogen Plasmodiophora brassicae infected its hosts and set up the parasitic relationship. We found the earlier the pathogent infected its host, the severer the disease was. Therefore, early control was the most effective. For Chinese cabbage, all controlling measures should be taken in the early 30 days because the new infection could not cause severe symptom after 30 days of seeding. For example, a biocontrol agent, Bacillus subtilis Strain XF-1 could control the disease 70%-85% averagely when it mixed with seedling substrate and was drenching 3 times after transplanting, i.e. immediately, 7 days, 14 days. XF-1 has been deeply researched in control mechanisms, its genome, and development and application of biocontrol formulate. It could produce antagonistic protein, enzyme, antibiotics and IAA, which promoted rhizogenesis and growth. Its The genome was sequenced by Illumina/Solexa Genome Analyzer to assembled into 20 scaffolds then the gaps between scaffolds were filled by long fragment PCR amplification to obtain complet genmone with 4,061,186 bp in size. The whole genome was found to have 43.8% GC, 108 tandem repeats with an average of 2.65 copies and 84 transposons. The CDSs were predicted as 3,853 in which 112 CDSs were predicted to secondary metabolite biosynthesis, transport and catabolism. Among those, five NRPS/PKS giant gene clusters being responsible for the biosynthesis of polyketide (pksABCDEFHJLMNRS in size 72.9 kb), surfactin(srfABCD, 26.148 kb, bacilysin(bacABCDE 5.903 kb), bacillibactin(dhbABCEF, 11.774 kb) and fengycin(ppsABCDE, 37.799 kb) have high homolgous to fuction confirmed biosynthesis gene in other strain. Moreover, there are many of key regulatory genes for secondary metabolites from XF-1, such as comABPQKX Z, degQ, sfp, yczE, degU, ycxABCD and ywfG. were also predicted. Therefore, XF-1 has potential of biosynthesis for secondary metabolites surfactin, fengycin, bacillibactin, bacilysin and Bacillaene. Thirty two compounds were detected from cell extracts of XF-1 by MALDI-TOF-MS, including one Macrolactin (m/z 441.06), two fusaricidin (m/z 850.493 and 968.515), one circulocin (m/z 852.509), nine surfactin (m/z 1044.656~1102.652), five iturin (m/z 1096.631~1150.57) and forty fengycin (m/z 1449.79~1543.805). The top three compositions types (contening 56.67% of total extract) are surfactin, iturin and fengycin, in which the most abundant is the surfactin type composition 30.37% of total extract and in second place is the fengycin with 23.28% content with rich diversity of chemical structure, and the smallest one is the iturin with 3.02% content. Moreover, the same main compositions were detected in Bacillus sp.355 which is also a good effects biocontol bacterial for controlling the clubroot of crucifer. Wherefore those compounds surfactin, iturin and fengycin maybe the main active compositions of XF-1 against P. brassicae. Twenty one fengycin type compounds were evaluate by LC-ESI-MS/MS with antifungal activities, including fengycin A $C_{16{\sim}C19}$, fengycin B $C_{14{\sim}C17}$, fengycin C $C_{15{\sim}C18}$, fengycin D $C_{15{\sim}C18}$ and fengycin S $C_{15{\sim}C18}$. Furthermore, one novel compound was identified as Dehydroxyfengycin $C_{17}$ according its MS, 1D and 2D NMR spectral data, which molecular weight is 1488.8480 Da and formula $C_{75}H_{116}N_{12}O_{19}$. The fengycin type compounds (FTCPs $250{\mu}g/mL$) were used to treat the resting spores of P. brassicae ($10^7/mL$) by detecting leakage of the cytoplasm components and cell destruction. After 12 h treatment, the absorbencies at 260 nm (A260) and at 280 nm (A280) increased gradually to approaching the maximum of absorbance, accompanying the collapse of P. brassicae resting spores, and nearly no complete cells were observed at 24 h treatment. The results suggested that the cells could be lyzed by the FTCPs of XF-1, and the diversity of FTCPs was mainly attributed to a mechanism of clubroot disease biocontrol. In the five selected medium MOLP, PSA, LB, Landy and LD, the most suitable for growth of strain medium is MOLP, and the least for strains longevity is the Landy sucrose medium. However, the lipopeptide highest yield is in Landy sucrose medium. The lipopeptides in five medium were analyzed with HPLC, and the results showed that lipopeptides component were same, while their contents from B. subtilis XF-1 fermented in five medium were different. We found that it is the lipopeptides content but ingredients of XF-1 could be impacted by medium and lacking of nutrition seems promoting lipopeptides secretion from XF-1. The volatile components with inhibition fungal Cylindrocarpon spp. activity which were collect in sealed vesel were detected with metheds of HS-SPME-GC-MS in eight biocontrol Bacillus species and four positive mutant strains of XF-1 mutagenized with chemical mutagens, respectively. They have same main volatile components including pyrazine, aldehydes, oxazolidinone and sulfide which are composed of 91.62% in XF-1, in which, the most abundant is the pyrazine type composition with 47.03%, and in second place is the aldehydes with 23.84%, and the third place is oxazolidinone with 15.68%, and the smallest ones is the sulfide with 5.07%.

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The Factors for the Formation of Carcinogenic N-Nitrosamine from Dried Marine Food Products (수산 건제품중 발암성 N-NITROSAMINE의 생성 요인)

  • SUNG Nak-Ju;KANG Shin-Kwon;LEE Soo-Jung;KIM Sung-Hee
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.27 no.3
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    • pp.247-258
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    • 1994
  • A total of 31 commercial dried marine food products, consisting of 14 fishes, 2 shellfishes and 2 seaweeds species were analyzed for their contents of precusors of N-nitrosamine such as dimethylamine(DMA), trimethylamine(TMA), trimethylamine oxide (TMAO), betaine and nitrate and nitrite nitrogen as factors of N-nitrosamine formation. Carcinogenic N-nitrosamines were extracted by a steam distillation apparatus and were analyzed for their components using a gas chromatography-thermal energy analyzer. N-nitrosodimethylamine(NDMA) was confirmed by a gas chromatography-mass spectrometry. The contents of betaine nitrogen in samples were in the range of $5.2{\sim}373.8mg\%$ and were significantly higher than tertiary amines such as TMA and TMAO. DMA nitrogen in those samples was in the range of trace-31.2ppm and was high, in the dried shark(31.2ppm), alaska pollack($22.9{\sim}24.3ppm$) and octopus($17.9{\sim}18.4ppm$). In dried laver and sea mustard, however, amines were not detected at all. The levels of nitrate nitrogen in the dried marine samples ranged from zero to 16.8ppm and were high in the dried stingray(16.8ppm), alaska pollack(16.3ppm) and squid($2.2{\sim}12.4ppm$), but were less than 1.0 ppm in other samples. The levels of nitrite nitrogen were lower than those of nitrate nitrogen and it was not detected in dried sea cucumber, laver and sea mustard. Twenty eight of 31 samples contained NDMA($range=1.2{\sim}86.0ppb$), which was the only volatile N-nitroso compound found. The NDMA levels of dried stingray($2.8{\sim}86.0ppb$), alaska pollack($8.2{\sim}55.5ppb$), squid($3.3{\sim}53.2ppb$), yellow corvenia($45.9ppb$) and plain dried shrimp($15.4{\sim}17.9ppb$) were high. However, it was not detected in dried sea cucumber, laver and sea mustard. Samples, containing high levels of NDMA, also contained high nitrate and nitrite nitrogen. From above results, it can be concluded that nitrate and nitrite were major factors for the formation of NDMA in dried marine food products.

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Monitoring of Hazardous Chemicals for Effluents of STPs and WWTP in the Nakdong River Basin (낙동강수계 주요 하·폐수처리장 방류수내 미량유해물질 모니터링)

  • Kim, Gyung-A;Seo, Chang-Dong;Lee, Sang-Won;Ryu, Dong-Choon;Kwon, Ki-Won
    • Journal of Environmental Science International
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    • v.23 no.7
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    • pp.1253-1268
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    • 2014
  • This study was investigated twenty two hazardous chemicals compounds for effluents of nine sewage treatment plants (STPs) and one waste water treatment plant (WWTP) in the Nakdong Ri-ver Basin. They are eleven phthalates(DMP, DEP, DIBP, DBP, BEEP, DNPP, DHP, DCP, DEHP, DNOP, Dinonyl phthalate, seven aliphatic hydrocarbons(n-Tridecane, n-Tetradecane, n-Pentadecan-e, n-Hexadecane, n-Heptadecane, n-Octadecane, n-Nonadecane, Isoquinoline, 2-Chloropyridine, 2-N-itrophenol, and Benzophenone. The twenty two compounds were analyzed by gas chromatograp-hy mass spectrometry (GC/MS) with liquid-liquid extraction (LLE). Twenteen of twenty two subs-tances were detected. They were DMP, DEP, DIBP, DBP, DEHP, n-Tetradecane, n-Pentadecane, n-Heptadecane, n-Octadecane, n-Nonadecane, Isoquinoline and Benzophenone. Among these, DEHP, DEP and Benzophenone were most frequently observed. They were obtained as $ND{\sim}36.881{\mu}g/L$, $ND{\sim}0.950{\mu}g/L$, $ND{\sim}2.019{\mu}g/L$, respectively. When the substances were calculated the average concentration at 10 points, the maximum average detection concentration was investigated at the Dalseocheon STP.