• 농업과학연구
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• 제43권4호
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• pp.634-640
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• 2016

The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

• 한국환경보건학회지
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• 제32권2호
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• pp.164-170
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• 2006

Ethylene oxide is a genotoxic carcinogen with widespread uses as industrial chemical intermediate and gaseous sterilant. 2-hydroxyethylated N-terminal valine in Hb is a good biomarker for biological monitoring of ethylene oxide exposure, because of its stability. For measuring the hemoglobin adduct formed by exposure of ethylene oxide, we studied the determination of (N-2-hydroxy-ethyl)valine(HEV) in hemoglobin adduct by using GC/MS. Firstly we synthesized HEV with 2-amino-ethanol and bromoisovaleric acid(BIVA) and confirmed it with GC/MS-FID. Its fragmentations were m/z 116(base ion, M+-45) and m/z 130(M+-31). For measuring HEV with higher sensitivity, we use derivatives which were PFPITH(pentafluorophenylisothiocianate) and TBDMS (tributyldimethylsilylation) by using Edman procedure. Its fragmentation were m/z 425(M+-57), m/z 383(M+-99) and m/z 172(M+-310) by using GC/MS. We did biological monitoring for mice inhalation exposure with 400 ppm ethylene oxide. The concentrations of hemoglobin adduct were $168{\pm}3.8\;and\;512{\pm}04$(nmol g-1 globin) at 0.5 hr/day 400 ppm ethylene oxide inhalation exposure group, and $631{\pm}17\;and\;2265{\pm}9.4$(nmol g-1 globin) at 1.0 hr/day 400 ppm ethylene oxide inhalation exposure for 1 and 4 weeks, respectively. We confirmed that (N-2-hydroxy-ethyl)valine(HEV) of hemoglobin was a good biomarker for biomonitoring of ethylene oxide exposure, and can measured with derivatives such as PFPITH(pentafluorophenylisothiocianate) and TBDMS(tributyldimethylsilylation) by using GC/MS.

• 한국식품영양과학회지
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• 제36권2호
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• pp.201-208
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• 2007

홍국쌀을 $35^{\circ}C$, 175 rpm에서 80% ethanol을 이용하여 0.5, 1, 2, 4, 8, 24시간 단위로 개별적으로 에탄올 추출한 결과, 1시간(yield, 1.203%) 이후의 추출 시간 증가는 추출율의 증가에 큰 영향을 미치지 않았다. 1시간 추출한 홍국쌀 에탄올 추출물을 각각 600(A), 1200(B), 1800(C), 2280(D) ppm 함유하는 기능성 유지를 제조하였다. 기능성 유지의 색도는 추출물의 함유 농도가 높아짐에 따라 $L^*$ 값이 유의적으로 감소되며, $a^*$ 값 및 $b^*$ 값은 유의적으로 증가되는 경향을 나타내었다(p<0.05). 기능성 유지의 monacolin K 및 총 페놀 함량은 추출물 첨가량의 증가에 따라 유의적으로 증가되는 경향을 보였다(p<0.05). Rancimat$(98^{\circ}C)$ 분석을 실시한 결과, 기능성 유지의 induction time이 각각 control(4.3 hr), A(3.2 hr), B(2.6 hr), C(2.4 hr), D(2.2 hr)로 추출물 첨가 농도의 증가에 따라 다소 감소하는 경향을 나타내어 산화 안정성의 보강이 필요할 것으로 판단된다. 전자코에 의해 얻어진 각 시료의 센서의 감응도$({\Delta}R/R_0)$를 이용한 주성분분석 및 MANOVA 분석 결과, 제1주성분 기여율은 99.66%로 분석되었으며 함유된 추출물의 함량 증가에 따라 각각 차별적인 향 패턴(odor difference)을 보이는 것으로 확인되었다. SPME-GC/MS에 의한 휘발성분 분석 결과, 기능성 유지에서 홍국쌀 에탄올 추출물로부터 기인되는 특유의 휘발성분은 관찰되지 않았으나, RT=12.1 min인 hexanal의 함량이 control에 비하여 유의적인 감소 경향을 나타내는 것이 확인되었다(p<0.05).

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.3114-3114
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• 2001

During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

• 분석과학
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• 제20권4호
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• pp.315-322
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• 2007

본 연구는 1명의 건강한 성인남자로부터 pseudoephedrine과 dextromethorphan 복합제제 약물의 복용 후 24시간동안 배설된 소변을 채취하여 이들 혼합약물의 대사과정과 배설에 관하여 연구를 수행 하였다. 소변 중에 약물과 대사체의 검출을 위하여 가수분해 및 추출과정을 거쳐 MSTFA와 MBTFA를 사용하여 유도체 반응 후 GC-MS로 동시 분석을 수행하였다. 각 대사체는 질량스펙트럼의 해석을 통하여 구조가 규명되었으며, 시간에 따른 모 약물과 대사체의 배설율을 조사하였으며, 본 실험결과로부터 pseudoephedrine과 dextromethorphan의 체내 대사경로를 제안하였다.

• 한국연초학회지
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• 제19권1호
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• pp.57-63
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• 1997

The composition of leaf surface lipid in Flue-cured tobacco and their changes during curing was investigated. The flue-cured variety, Nicotiana tabacum cv. NC 82 was cultivated at Eumsung experiment station in 1996. The samples of riced leaves with different stalk Position(Lugs, Cutter, Leaf and Tips) and different curing stage at half yellowing(24hr), yellowing(48 hr) , color axing(72 hr), midrib drying(96 hr) and cured(120 hr) were collected for analysis of leaf surface lipid. $\alpha$ - and $\beta$ - 4, 8, 13-Duvatriene-1, 3-diol($\alpha$, $\beta$-DVT) were major components in leaf surface lipid extracted with methylene chloride and sugar ester was detected slightly DVT content was increased with ascending stalk position, but increasing trend of total hydrocarbon was not observed. While DVT was decreased throughout curing of tobacco leaves, hydrocarbon content did not show significant change during curing process. Twenty-two duvane compounds were detected by capillary GC in duvane fraction isolated from leaf surface lipid and of which 11 compounds were identified by GC-MS. These compounds were decreased with curing in all stalk position.

• 한국환경성돌연변이발암원학회지
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• 제21권2호
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• pp.122-127
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• 2001

4-tert-octylphenol (OP) is a surfactant additive widely used in the manufacture of a variety of detergents and plastic products. Also, OP is known to have estrogenic activity by interacting with development and functions of endocrine system. This study was carried out to obtain toxicokinetic parameters of OP in male Sprague-Dawley rats. Male rats were administered OP, by either single oral (gavage) applications of 50, 100 or 200 mg/kg body weight. or a single intravenous injections of 1, 5 or 10 mg/kg body weight. Blood samples taken at several time intervals after administration were obtained from the femoral artery. Analysis of blood samples for OP was performed by gas chromatography mass spectrometry (GC/MS). The detection limit of OP was 1.9 ng/$m\ell$ at SIM (selected ion monitoring) mode of GC/MS. Calibration curve for analysis of the concentrations of OP in plasma was (OP/butylphenol peak area ratio) = 0.0294 $\times$ (plasma cone.) + 0.028 ($r^2$= 0.9991). The OP plasma concentration was 3921 ng/$m\ell$ immediately after single intravenous application, decreased rapidly within 45 min, and was detectable at low concentration up to 6 hr after application. When administered orally in rats (50, 100 and 200 mg/kg), OP was detected in the blood early after gavage administration, indicating the rapid initial uptake from gastrointestinal tract, with Tmax obtained from 0.67~0.83 hr. Using the AUC (area under the curve) of plasma concentration vs. time, low oral bioavailabilities of 1.2, 5.0 and 5.3% were calculated for the 50, 100 and 200 mg/kg groups, respectively.

• 한국응용곤충학회지
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• 제45권2호
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• pp.189-194
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• 2006

털두꺼비하늘소(Moechotypa diphysis) 성충에 대한 18종 식물정유의 훈증독성을 조사하였다. 그들 중 10 $\mu\ell/\ell$ (공기)의 농도에서 eucalyptus oil, rosemary oil, 그리고 pennyroyal oil은 100%, sage oil은 85%의 살충활성을 나타내었다. 4종 정유의 치사속도를 조사한 결과, eucalyptus oil과 rosemary oil이 처리 후 6시간 이내에 100%의 살충률을 나타내었다. 각 정유에 대한 주요 구성성분을 GC와 GC/MS로 분석한 결과, eucalyptus oil, rosemary oil, sage oil의 주성분인 1,8-cineole과 sage oil의 또 다른 주성분인 thujone과 pennyroyal의 주성분인 pulegone 모두 20 $\mu\ell/\ell$(공기)의 농도에서 100%의 살충효과를 나타내었다.

• 분석과학
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• 제24권2호
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• pp.142-149
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• 2011

Resveratrol을 GC/TOF-MS를 이용하여 대사체를 확인한 결과, 두 개의 phenyl기를 연결하는 이중결합이 단일결합으로 환원된 구조로 추정되었다. 또한, GC/MSD를 이용하여 resveratrol 및 내인성스테로이드의 분석법에 대한 유효성을 점검한 결과, 회수율은 96.47 - 114.74%의 범위로 나타났으며, intra-day와 inter-day의 정밀도는 1.40 - 10.87%과 1.10 - 10.93% 그리고 정확도는 80.03 - 119.92%과 80.02 - 119.56%로 조사되었고, 모두 0.996이상의 직선성을 나타내어 유효한 분석 방법으로 검증되었다. 한편, 지원자들에게 resveratrol을 경구투여 한 요시료로부터 resveratrol과 그 대사체에 대한 상관성을 조사해본 결과, 요중 최대농도 도달시간이 일반적인 약물(1 - 2시간) 보다 긴 10 - 15시간에 나타났으며, 대사체로의 전환율은 남성보다 여성이 높게 나타났다. 한편, 내인성 스테로이드는 약물 복용 후 20시간 까지는 resveratrol 및 그 대사체와 다소 유사한 분비형태를 나타내었으며, estrone과 estradiol의 경우 여성이 남성에 비해 이 약물에 대한 민감성이 높게 나타났다. 그 외의 내인성 스테로이드는 유의할만한 차별된 분비형태의 변화가 나타나지 않았다. 따라서 resveratrol의 경우 약물의 활성이 남성보다는 여성에게 유의한 영향을 미치는 것으로 추측되었다.

• 분석과학
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• 제17권2호
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• pp.117-129
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• 2004

본 연구에서는 극성이 높고, 휘발성이 낮아 GC나 GC/MS로 분석이 곤란한 환경매체 중의 아미트롤을 LC/ESI/MS를 사용하여 분석한 결과 다음과 같은 결론을 얻었다. 분자량이 84인 아미트롤은 LC/ESI/MS 방식에서는 m/z 85인$(M+H)^+$형태로 나타났으며, 피크강도는 30V에서 (SIR mode) 최대를 나타내었다. 질량 스펙트럼 비를 정성확인에 적용하기 위하여 실험한 결과 아미트롤은 m/z 85 와 m/z 58 이온으로 나타났으며, 50V에서 이 비는 1 : 7.03~7.58 로 나타났다. 동위원소 비를 이용한 정성확인은 isotope MS나 HR/MS가 주로 사용되나, 본 연구에서는 정성확인을 위한 보조수단으로 이용하고자 실험한 결과 아미트롤의 동위원소는 $86([M+H])^+$ 형태로 나타났으며, 시료에서(30V) m/z 85와 m/z 86의 질량 스펙트럼 비는 27.1~28.6 : 1(이론적 비 26.6 : 1)로 나타났다. 단계별 표준액을 시료의 전 처리 방법과 동일하게 처리하여 분석한 검량선의 직선성은 $y=1.09354e^6X+26947.2$이었으며, $r^2=0.99$로 나타났다. 분석의 정도관리를 위한 회수율검정과 반복 재현성을 알아보기 위한 실험에서 수질시료의 회수율은 77.64~83.44%, 토양시료에서는71.11~79.44%로 나타났으며, 각 농도 단계별 반복(5회)실험결과 상대표준편차 값은 10%이하를 나타내었다.