• 제목/요약/키워드: GC-determination

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Occurrence and risk assessment of phenol and substituted phenols in water and fish collected from the streams in eastern Gangwon State, Korea

  • Sunyoung Park;Jaeseok Choi;Jaeyong Lee;Hekap Kim
    • 분석과학
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    • 제36권5호
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    • pp.224-235
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    • 2023
  • An analytical method was developed for the determination of phenol (P) and the seven substituted phenols in water samples and fish tissue samples collected from three streams located in eastern Gangwon State in spring and summer. The phenols were extracted and then derivatized to phenyl acetates using acetic anhydride. The derivatives were subsequently identified and quantified using gas chromatography coupled with mass spectrometry. P and 4-nitrophenol (4NP) were found at relatively high levels in water, ranging from below the method detection limit (MDL) to 3.32 ㎍/L and from < MDL to 4.91 ㎍/L, respectively. P and 4NP were also the dominant compounds in the fish tissue, ranging from < MDL to 407 ㎍/kg and from < MDL to 870 ㎍/kg, respectively. Phenol concentrations were significantly higher in spring than in summer. The ecological risk quotient calculated for P was higher than 4NP but not high enough to pose any risk of adverse effects to fish health.

포도당, 젖산 및 에탄올의 동시 측정용 바이오센서의 개발 (Development of Biosensor for Simultaneous Determination of Glucose, Lactic Acid and Ethanol)

  • 김정호;이동희;김태진;노봉수
    • 한국식품과학회지
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    • 제30권1호
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    • pp.22-34
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    • 1998
  • 고정화효소와 산소전극 시스템을 이용한 효소센서를 제작하여 식품 중의 당, 유기산, 알코올 성분을 동시 측정 하였다. 효소가 기질과 반응하여 소비한 산소의 변화량이 전압차이로 나타나므로 시간당 전압 감소량이 최대인 값으로부터 각 성분의 농도를 측정하였으며, 이때 1분내에 최대기울기를 구할 수 있어 신속한 측정이 가능하였다. 효소의 고정화 지지체로는 nylon cloth를 사용하였고, asymmetrical coupling 방법에 의하여 기질 작용 순으로 위치하도록 효소를 고정화하였다. 한 개의 양극과 6개의 음극으로 제작된 multiple cathode system으로 포도당, 젖산, 에탄올 성분을 동시 측정할 수 있는 효소 센서를 제작하였다. 위의 센서 제작을 위하여 mutarotase과 glucose oxidase/lactate oxidase/alcohol oxidase와 catalase가 각기 사용되었다. 이들 효소센서의 최적조건은 $pH\;7.0,\;40^{\circ}C$의 0.1 M 인산완충용액이었으며 각 효소 센서의 방해물질을 알아 보기 위하여 여러 가지 당과 각종 유기산, 알콜류에 대한 효소 감응도를 살펴 본 결과 포도당 센서에서 유기산의 영향을 제외하고는 10% 내외였다. 따라서 포도당과 유기산을 동시 측정하기 위하여 포도당/젖산의 영향을 고려한 적절한 보정관계식을 도입하여 순수한 유리당과 유기산의 값을 측정할 수 있었다. 제작된 효소센서의 검증을 위하여 분광광도법. HPLC, GC를 이용한 결과, 분석방법간에 높은 상관관계를 보여 주었다. 아울러 각 효소센서의 안정성을 살펴본 결과 알코올 센서를 제외하고는 30일 이후에도 80%이상 효소감응도가 유지되었다.

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도파민으로 수식된 3,4-dihydroxybenzoic acid 고분자 피막전극을 이용한 Ti(IV)이온의 정량 (Poly-3,4-dihydroxybenzoic Acid Film Electrodes Modified with Dopamine for Determination of Ti(IV) Ions)

  • 차성극
    • 전기화학회지
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    • 제6권2호
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    • pp.130-133
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    • 2003
  • 3,4-dihydroxybenzoic acid(3,4-DHBA)를 전기화학법으로 유리탄소 전극 위에 중합하여 GC/p-3,4-DHBA형의 전극을 제작한 후 이 전극을 도파민으로 재 수식한 전극을 제작하였다. 이 때 고분자 피막 상에 카르복시기와 도파민의 아민 기간에 짝 짓기 반응은 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride(EDC)의 존재하에서 진행되었다. 이 반응과정에서 반응한 도파민의 양은 수정판 분석기(quartz crystal analyzer:QCA)에 의하여 결정하였으며 그때 전극형태는 QCA(Au)/p-3,4-DHBA-dopamine이었다. 이 전극의 표면은 o-퀴논부분을 갖고 있어서 티탄이온에 선택성이 큰 특성을 갖고 있다. 이 전극의 산화환원과정은 $hydroquinone = quinone +2H^+2e^-$으로 두 개의 강한 파와 두개의 약한 파가 CV과정에서 관찰되었다. 이 수식전극으로 Ti(IV)이온을 $4.13\times10^{-5} gcm^{-2}$만큼 포집할 수가 있었다. 이 수식 전극으로 $5.25\times10^{-4}M$에서 $5.25\times10^{-8}M$농도범위까지 정량 할 수 있는 상관계수가 0.997인 검정선을 얻었다.

카리소프로돌 중독사의 치사혈중농도 및 조직분포 (Postmortem Blood and Tissue Concentration of Carisoprodol and Meprobamate)

  • 최혜영;최화경;이주선;우상희;이한선;박유신;정희선
    • 대한임상독성학회지
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    • 제1권1호
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    • pp.34-39
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    • 2003
  • Carisoprodol (CSP) is commonly prescribed as a skeletal muscle relaxant. Recently, we encountered 7 suicidal cases in which carisoprodol was detected. We developed a rugged, sensitive, and specific method for the determination of CSP and meprobamate (MPB) by GC and GC/MS. Postmortem blood concentrations of CSP and MPB ranged 22.9-124.4 ,$\mu$g/ml and its metabolite, 26.8-144.5 ,$\mu$g/ml respectively. Among 7 cases studied, Only CSP was ingested in 4 cases and combination of CSP and dextromethorphan was ingested in 2 cases according to the case history and one case was with ethanol. The order of the tissue concentration of CSP and MPB was liver> kidney > brain, and the concentration of MPB was higher than that of CSP in all tissues. The MPB /CSP concentration ratios of urine, bile juice, liver, kidney, brain and blood were 15.7, 4.0, 1.2, 1.4, 1.4 and 1.0 respectively. There was a big difference in concentration of CSP and MPB in 7 cases due to differences in the amount of dose administered and time to death after dosing.

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환경대기 중 프탈레이트 화합물의 농도 측정 (II) - 실험재료 전처리 및 시료정제과정 평가 - (Determination of Phthalates Compounds in the Ambient Atmosphere (II) - Evaluation of Experimental Artifacts and Sample Clean-up Procedures -)

  • 박영화;황윤정;서영교;백성옥
    • 대한환경공학회지
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    • 제32권5호
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    • pp.455-460
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    • 2010
  • 본 연구에서는 프탈레이트 화합물 측정 시 시료채취 및 분석과정 증에서 야기될 수 있는 공시료의 오염여부를 평가하고 clean-up 절차와 같은 적절한 개선 방안을 제시하였다. 실험도구 및 시료채취 매체에 대한 공시료를 평가한 결과 많은 종류의 실험기구 및 장치에서 DBP와 DEHP가 잔존하는 것으로 나타났다. 따라서 실험도구는 반드시 전처리하여 사용해야 하며, 이후 공시료 보정이 수반되어야 한다. 또한 본 연구에서 제시한 clean-up 방법을 통해 불순물이 많이 제거되었으며, GC/MS를 이용한 정성?정량분석에서 정도개선에 효과적인 것으로 나타났다.

흡착튜브 - 열탈착 정량분석 기법에 기반한 과일시료로부터 자연적 휘발성유기화합물의 배출특성 연구 (Biogenic Volatile Organic Compounds (BVOC) Emissions from Fruit Samples Based on Sorbent Tube Sampling and Thermal Desorption (ST-TD) Analysis)

  • 안정현;김기현
    • 한국대기환경학회지
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    • 제29권6호
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    • pp.757-772
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    • 2013
  • In this study, a combination of sorbent tube (ST)-thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) was used for quantitative analysis of liquid phase standards of 10 BVOC ((1) (+)-${\alpha}$-pinene, (2) (+)-${\beta}$-pinene, (3) ${\alpha}$-phellandrene, (4) (+)-3-carene, (5) ${\alpha}$-terpinene, (6) p-cymene, (7) (R)-(+)-limonene, (8) ${\gamma}$- terpinene, (9) myrcene, and (10) camphene). The results of BVOC calibration yielded comparatively stable pattern with response factor (RF) of 23,560~50,363 and coefficient of determination ($R^2$) of 0.9911~0.9973. The method detection limit (MDL) of BVOC was estimated at 0.03~0.06 ng with the reproducibility of 1.30~5.13% (in terms of relative standard error (RSE)). Emissions of BVOC were measured from four types of fruit samples ((1) tangerine (TO), (2) tangerine peel (TX), (3) strawberry (SO), and (4) sepals of strawberry (SX)). The sum of BVOC flux (${\sum}flux$ (BVOC) in ng/hr/g) for each sample was seen on the descending order of (1) TX=291,614, (2) TO=2,190, (3) SO=1,414, and (4) SX=2,093. If the results are compared between the individual components, the highest flux was seen from (R)-(+)-limonene (265,395 ng/hr/g) from TX sample.

사과 성숙(成熟) 및 저장중(貯藏中) 향기성분(香氣成分)의 변화(變化) -제일보(第一報). 과실(果實) 성숙중(成熟中) 향기성분(香氣成分)의 동정(同定) 및 정량(定量)- (Changes of Volatiles from Apple Fruits during Maturity and Storage -Part. I. Identification and Determination of Volatiles in the Fruits-)

  • 심기환;손태화;김명찬;강신권;박석규
    • Applied Biological Chemistry
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    • 제27권1호
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    • pp.14-20
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    • 1984
  • 우리 나라에서 비교적 생산량이 많은 사과과실 3품종(Fuji, 홍옥, 국광)을 대상으로 향기성분을 분리 및 동정하고, 또한 성숙시기별로 향기성분의 함량변화를 측정하였다. 향기성분은 30종 이상 분리되었고 그 중 ester 23종, alcohol 9종 및 aldehyde 2종을 동정하였다. 성숙중 향기성분의 종류와 함량은 증가하였으며 1-butanol, isobutyl butyrate, 2-pentanol, ethyl valerate 및 hexanal 등의 함량이 많았다.

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육류가공식품의 조리방법에 따른 PAHs 발생 특성에 관한 연구 (Characteristics of PAH Occurrence during Meat Cooking)

  • 이병호;안유진;박동윤;변기영;김경동;이미림;서정범;박은영;박흥재
    • 한국환경과학회지
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    • 제25권11호
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    • pp.1459-1466
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    • 2016
  • In this study, the concentrations of polycyclic aromatic hydrocarbons (PAHs) were investigated in meat process food and for cooking methods (pan-frying and charcoal fire). The methodology involved liquid-liquid extraction, silica gel cartridge clean-up and determination by gas chromatography/mass spectrometry (GC/MS). The recovery of 17 PAHs spiked into these samples ranged from 66.6 % to 98.0% and the coefficient of variation was less than 10%, but that of dibenz(a,h)anthracene was 16.39%. The mean concentration of total PAHs in processed samples was ND~7.2 ng/g, whereas that pan-fried and charcoal-fired samples were ND~22.1 ng/g and, 12.7~367.8 ng/g, respectively. Therefore, the concentrations of total PAHs in cooked samples were higher than in original samples and charcoal-fired samples had the highest total PAH levels.

Validation and Recommendation of Methods to Measure Biogas Production Potential of Animal Manure

  • Pham, C.H.;Triolo, J.M.;Cu, T.T.T.;Pedersen, L.;Sommer, S.G.
    • Asian-Australasian Journal of Animal Sciences
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    • 제26권6호
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    • pp.864-873
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    • 2013
  • In developing countries, biogas energy production is seen as a technology that can provide clean energy in poor regions and reduce pollution caused by animal manure. Laboratories in these countries have little access to advanced gas measuring equipment, which may limit research aimed at improving local adapted biogas production. They may also be unable to produce valid estimates of an international standard that can be used for articles published in international peer-reviewed science journals. This study tested and validated methods for measuring total biogas and methane ($CH_4$) production using batch fermentation and for characterizing the biomass. The biochemical methane potential (BMP) ($CH_4$ NL $kg^{-1}$ VS) of pig manure, cow manure and cellulose determined with the Moller and VDI methods was not significantly different in this test (p>0.05). The biodegradability using a ratio of BMP and theoretical BMP (TBMP) was slightly higher using the Hansen method, but differences were not significant. Degradation rate assessed by methane formation rate showed wide variation within the batch method tested. The first-order kinetics constant k for the cumulative methane production curve was highest when two animal manures were fermented using the VDI 4630 method, indicating that this method was able to reach steady conditions in a shorter time, reducing fermentation duration. In precision tests, the repeatability of the relative standard deviation (RSDr) for all batch methods was very low (4.8 to 8.1%), while the reproducibility of the relative standard deviation (RSDR) varied widely, from 7.3 to 19.8%. In determination of biomethane concentration, the values obtained using the liquid replacement method (LRM) were comparable to those obtained using gas chromatography (GC). This indicates that the LRM method could be used to determine biomethane concentration in biogas in laboratories with limited access to GC.

Quantitative Analysis of Cinnamaldehyde, Cinnamylalcohol and Salicylaldehyde in Commercial Biopesticides Containing Cinnamon Extract Using Gas Chromatography - Flame Ionization Detector

  • Lim, Sung-Jin;Lee, Ji-Hye;Kim, Jin-Hyo;Choi, Geun-Hyoung;Cho, Nam-Jun;Park, Byung-Jun
    • 한국환경농학회지
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    • 제33권3호
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    • pp.213-219
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    • 2014
  • BACKGROUND: In an environment-friendly agriculture, plant extracts have been perceived as alternatives of synthetic pesticides. The Environment-friendly Agriculture Promotion Act of Korea has approved cinnamon extract as a matter for the production of commercial biopesticides. Thirteen commercial biopesticides containing cinnamon extract have been marketed locally. However, the analytical method for the quality control of these biopesticides containing cinnamon extract has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of cinnamaldehyde, cinnamylalcohol and salicylaldehyde in biopesticides containing cinnamon extract was developed and validated by gas chromatography (GC). The clean-up method was optimized with HLB SPE cartridges for the bioactive substance in biopesticides containing cinnamon extract, and the eluate was analyzed by GC. The developed method was validated, and the LOQ and recovery rates of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were 0.139, 0.067 and $0.062mgL^{-1}$ and 84.2, 86.5 and 82.1%, respectively. The contents of cinnamaldehyde, cinnamylalcohol and salicylaldehyde were analyzed using the developed method in the 13 commercial biopesticides. Results showed 0.06-17.37%,