• 분석과학
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• 제14권2호
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• pp.95-102
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• 2001

쇠고기 돼지고기 속에 포함된 nonylphenol, octylphenol, bis(2-ethyltexyl) phthalate의 동시 정량방법을 연구하였다. 이 방법에서는 밀폐된 배양시험관에서 이염화메탄을 이용하여 추출하고 용매를 이소헥산으로 바꾸고 aminopropyl 칼럼(2g)을 이용하여 분리한 후 GC/MS-SIM 방법으로 분석하였다. 다중점보정을 위한 nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl) phthalate(BEHP)의 회수율에서 NP, OP는 $0.125-12.5{\mu}g/g$, BEHP는 $0.0125-12.5{\mu}g/g$ 범위에서 좋은 회수율을 보였다. 확립된 방법을 전주시와 전주시 근교 마트와 정육점에서 구입한 16점의 쇠고기 돼지고기 시료에 적용하였다. Nonylphenol은 4점의 시료에서 검출되었으며 bis(2-ethlhexyl) phthalate는 전 시료에서 검출되었고, 그 농도범위는 $0.06-0.24{\mu}g/g$과 $0.36-2.35{\mu}g/g$ 이었다. Octylphenol은 어떠한 시료에서도 검출되지 않았다. 이 방법은 매우 적은량의 생체 시료에도 쉽게 적용이 가능하였다.

• 한국축산식품학회지
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• 제30권1호
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• pp.73-86
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• 2010

The current study was designed to optimize solid phase microextraction (SPME)-GC-MS conditions for extraction and analysis of volatile components for Hanwoo beef and to establish a tentative database of flavor components. Samples were taken from Hanwoo longissimus muscle (30 mon old steer, $1^+B$ carcass grade) at 24 h postmortem. Results indicated that the optimum adsorption time for $75{\mu}m$ CAR/PDMS fiber was 60 min at $60^{\circ}C$. Thermal cleaning at $250^{\circ}C$ for 60 min was the best practice for decontamination of the fiber. A short analysis program with a sharp oven temperature ramp resulted in a better resolution and higher number of measurable volatile components. With these conditions, 96 volatile compounds were identified with little variation including 22 aldehydes, 8 ketones, 31 hydrocarbons, 12 alcohols, 8 nitrogen- and sulfurcontaining compounds, 5 pyrazines and 10 furans. A noticeable observation was the high number of hydrocarbons, aldehydes, ketones, alcohols and 2-alkylfurans which were generated from lipid decomposition especially the oxidation and degradation of unsaturated and saturate fatty acids. This implies that these compounds can be candidates for flavor specification of highly marbled beef such as Hanwoo flavor.

• 대한화학회지
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• 제41권9호
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• pp.471-482
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• 1997

기체크로마토그래피/질량분석법(GC/MS)을 이용하여 소변 내에 존재하는 유기산들을 동시에 분리 정량분석할 수 있는 최적의 분석조건을 확립하기 위해 액체-액체추출법을 이용하여 분리하였고 이 때 pH의 영향 및 역추출방법과 그리고 옥심화 과정 첨가의 효과를 알아보았다. 그 결과 옥심화 과정 없이 pH가 0.5일 때 회수율이 좋았고 RSD값은 0.3-12.4%로 가장 적었다. 역추출과정을 통하여 방해물질이 제거되어 15-16분대의 머무름 값을 갖는 몇가지 유기산 검출이 확실시 되었다. 이를 토대로 51종의 유기산들에 대한 검량곡선을 작성하여 한국 정상어린이(n=16) 요시료 중의 유기산 함량분포를 얻었다.

• 한국환경과학회지
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• 제13권5호
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• pp.469-478
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• 2004

Atmospheric bulk (wet and dry) samples were monthly collected in an urban environment (Daeyeon-dong) of Busan over a year, to assess the deposition flux and seasonality of dioxin-like polychlorinated biphenyls (DLPCBs) using stainless steel pots. Deposition fluxes of DLPCBs in bulk samples were determined using high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Particle deposition fluxes in the urban environment varied from 23 to 98 $mg^2$/year (mean 41 $gm^2$/year). DLPCB deposition fluxes in atmospheric bulk samples ranged from 0.09 to 0.77 ng-$TEQ/m^2$/year (mean 0.35 ng-$TEQ/m^2$/year). Seasonal atmospheric deposition fluxes of DLPCBs were high in winter and low in summer. Atmospheric deposition fluxes of particles and DLPCBs in this study were comparable to or slightly lower values than those of different locations in the world. Monthly DLPCB profiles in deposition bulk samples were similar over a year. Non-ortho PCBs were higher contributions to the total DLPCBs fluxes than mono-ortho PCBs. In particular, PCB 126 had the highest concentrartion (>75%) in all deposition samples, followed by PCB 169 and PCB 156. A highly positive correlation was found among the deposition fluxes of DLPCB species, suggesting the possibility of that the DLPCB contamination originated from one source. The deposition fluxes of DLPCBs were not significantly correlated with temperature and the amount of precipitation even though the summer season with the highest temperature and the largest amount of precipitation showed the lowest DLPCB deposition flux.

• 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.

• Bulletin of the Korean Chemical Society
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• 제23권2호
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• pp.225-228
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• 2002

Amorphous $Ga_2O_3$ films have been grown on Si(100) substrates by metal organic chemical vapor deposition (MOCVD) using gallium isopropoxide, $Ga(O^iPr)_3$, as single precursor. Deposition was carried out in the substrate temperature range 400-800 $^{\circ}C$. X-ray photoelectron spectroscopy (XPS) analysis revealed deposition of stoichiometric $Ga_2O_3$ thin films at 500-600 $^{\circ}C$. XPS depth profiling by $Ar^+$ ion sputtering indicated that carbon contamination exists mostly in the surface region with less than 3.5% content in the film. Microscopic images of the films by scanning electron microscopy (SEM) and atomic force microscopy (AFM) showed formation of grains of approximately 20-40 nm in size on the film surfaces. The root-mean-square surface roughness from an AFM image was ${\sim}10{\AA}$. The interfacial layer of the $Ga_2O_3$/Si was measured to be ${\sim}35{\AA}$ thick by cross-sectional transmission electron microscopy (TEM). From the analysis of gaseous products of the CVD reaction by gas chromatography-mass spectrometry (GC-MS), an effort was made to explain the CVD mechanism.

• 분석과학
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• 제12권2호
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• pp.151-158
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• 1999

국내 4대강 주요 하천 저니토양중 PCB 오염도를 각 congener별로 또는 총량으로서 GC/MS를 사용하여 정량하였다. 그 결과 4대강의 주요 지천중 SS지점 근처의 저니토에서 총 PCBs가 가장높은 $290.87{\mu}g/kg$이었고 OS지점에서도 비교적 높은 $221.11{\mu}g/kg$이었으며 저니중 유기물 함량과 상관관계가 있었다. Congener-specific analysis에 의해 하천수 및 저니토 시료에서 공통적으로 검출된 대표적 congener는 IUPAC No 66, 74, 90, 101, 105, 110, 118, 138, 149, 153, 180, 187였다. 본 연구결과 저니토에서는 tetraCBs 및 pentaCBs가 다른 polyCBs에 비해 비교적 높은 농도로 검출되었다. 이상의 연구결과를 통해 국내의 주요 하천의 저니토중 PCB의 오염정도는 매우 심각한 정도는 아니나 좀더 많은 시료를 분석하는 정말조사가 필요하다.

• 분석과학
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• 제7권1호
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• pp.65-78
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• 1994

제초제로 사용되고 있는 농약 중 트리아진류 7종과 에스텔화된 페녹시산류 9종의 혼합물을 기체 크로마토그래피/질량분석기(GC/MS)를 이용한 선택이온 검출법(SIM)으로 동시에 분리 및 정량하는 방법을 연구하였다. 수질에 잔류하는 농약들을 $CH_2Cl_2$로 추출, 농축 및 유도체화하여 GC/MS/SIM 방법으로 분석할 때 각종 농약류의 정량 농도 범위 0.2~5.0ng/ml에서 직선성이 양호하였고 검출한계는 0.2~0.5ng/ml 범위였다. 또한 이 분석방법을 음용수 또는 생체시료에도 적용 가능하였다.

• 한국식품위생안전성학회지
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• 제5권3호
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• pp.159-164
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• 1990

To detect and quantitation residual antibiotics and antibacterial agents in meats, we performed a biological assay employing the three microorganisms Bacillus subtilis ATCC 6633, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778 for the screening purpose and developed a Gas Chromatography-mass Spectrometry(GC/MS) analysis for the confirmation and quantiation. In the biological assay (paper disk method), three test solution are used depending on the character of the residual antibiotics and antibacterial agents, follow by a simple clean up procedure which includes homogenization with Mcilvaine buffer, defatting with includes homogenization with Mcilvaine buffer, defatting with hexane, extraction with chloroform, clean-up by Sep-Pak $C_{18}$ and Bakerbond SPE carboxylic acid column. The chloroform layer is used for the analysis of sulfa agents. macrolides antibiotics and antibacterial agents, Adsorbed materials in the Sep-Pak $C_{18}$ were also employed for th analysis of penicillins and tetracyclines. Effluents from the Sep-Pak $C_{18}$ were cleaned-up one more by Bakerbond 10 SPE COOH column and employed for the analysis of aminoglycosides. In the instrumental analysis by using the GC/MSD, residual antibiotics and antibacterial agent were quantitated by selected ion monitoring (SIM) mode after derivatization. A simultaneous analysis of six residual antibiotic and antibacterial agent such as oxytetracycline, penicillin, ampicillin, choliraphenicol and thiamphenicol was developed with simple cleanup procedures revealing good recovery and reproducibility. Also, simultaneous detection of macrolides antibiotics such as erythromycin, spiramycin, and oleandomycin was developed after acid hydrolysis due to their large molecular structures. Because of the high reproducibility and selectivity of these two methods, it is very desirable that the combination of the two methods be used in the bioassay for the screening of residual antibiotics and antibacterial agent and that GC/MSD analysis be used for the confirmation and quantitation.

• 대한수의학회지
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• 제48권1호
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• pp.39-48
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• 2008

Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) are ubiquitous and can contaminate the food chain. A study monitoring PCDD/Fs in imported meat was conducted at the National Veterinary Research and Quarantine Service (NVRQS, Republic of Korea) in order to maintain food safety from the bioaccumulative PCDD/Fs. Seventeen PCDD/Fs with toxic equivalency factors (TEFs) established by World Health Organization (WHO, 1998) were analyzed in imported beef, pork, and chicken by high resolution gas chromatography/mass spectrometry (HR-GC/MS). Results of the monitoring for the last 5 years are presented. The levels of PCDD/Fs were similar to other studies except two unusually high concentrations in pork and beef. Excessive levels greater than the Korean provisional maximum residue limit of PCDD/Fs were found in a sample of pork imported from Chile and a sample of beef imported from U.S, and those products were rejected and returned. There was no obvious trend or differences with respect to time or origin of meat in this study.