• Environmental Analysis Health and Toxicology
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• 제16권3호
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• pp.121-126
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• 2001

Analytical method of benzophenone (BP) in sediment and soil was developed by gas chromatography/mass selective detector/selected ion monitoring (GC/MSD/SIM). The ultrasonic extraction of US EPA (method 3550B) method and liquid-liquid extraction for sediment and soil samples were used for the analysis of BP from sediment and soil. BP was extracted with n-hexane. Organic layer was washed with 5% sodium chloride solution. 1∼2 l of the concentrated solution of organic layer was applied to GC/MSD. The retention time of BP peak was 11.10 min. Recovery (％) of BP by ultrasonication from sediment and soil samples was 96.0∼100.6％ and 40.0∼83.0％, respectively. Recovery of BP by liquid-liquid extraction was 51∼59％ in soil samples. The detection limit of BP in sediment and soil samples were determined to 0.1 ng/g.

• Environmental Engineering Research
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• 제13권4호
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• pp.216-223
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• 2008

An efficient method for the simultaneous determination of eleven phenolic endocrine-disrupting chemicals (EDCs) present in wastewater influent samples was described. The 11 phenolic EDCs including alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) following two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. The wastewater influent samples containing the 11 EDCs were adjusted to pH 2 with $H_2SO_4$ and then cleaned up with n-hexane. Next, they were subjected to solid-phase extraction (SPE) with XAD-4 resin and subsequently converted to isoBOC or TBDMS derivatives for sensitivity analysis with gas chromatography/mass spectrometry-selected ion monitoring (GC/MSSIM). Following isoBOC derivatization and TBDMS derivatization, the recoveries were 86.6-105.2% and 97.6-142.7%, the limits of quantitation (LOQ) for the 11 phenolic EDCs for SIM was 0.001-0.050 ng/mL and 0.003-0.050 ng/mL, and the SIM responses were linear with the correlation coefficient varying by 0.9717-0.9995 and 0.9842-0.9980, respectively. When these methods were applied to five selected wastewater influent samples, for isoBOC derivatization and TBDMS derivatization the ranges of concentration detected were 0.2-99.6 ng/mL and 0.4-147.4 ng/mL, respectively.

• Archives of Pharmacal Research
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• 제27권12호
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• pp.1295-1301
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• 2004

The enantiomeric composition tests on flurbiprofen and ketoprofen present in patch products and in urine excretions following patch applications were performed as diastereomeric (R)-(+)- 1-phenylethylamides by achiral gas chromatography and by gas chromatography-mass spectrometry in selected ion monitoring mode. The method for determination of (R)- and (S)-enantiomers in the range from 0.1 to 5.0 ${\mu}$g was linear (r ${\ge}$ 0.9996) with acceptable precision (% RSD ${\le}$5.2) and accuracy (% RE = 0.6 ~ -2.4). The enantiomeric compositions of flurbiprofen in one patch product and of ketoprofen in five different products were identified to be racemic with relatively good precision (${\le}$ 6.4%). The urinary excretion level of (R)-flurbiprofen was two times higher than its antipode, while the comparable excretion levels of (R)- and (S)-enantiomers for ketoprofen were observed.

• 분석과학
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• 제15권5호
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• pp.445-450
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• 2002

해수에 함유되어 있는 요오드화합물의 총량을 휘발성 유기물로 유도체화 후 측정하는 방법을 확립하였다. 이 방법은 요오드 음이온은 요오드로 산화시킨 후 2,6-dimethylphenol과 반응하여 4-iodo-2,6-dimethylphenol로 전환시켜 ethylether로 1단계 추출 후 gas chromatography-mass spectrometry (selected ion monitoring)로 측정하는 것으로 구성되어 있다. Iodate는 ascorbic acid 와 acetic acid로 요오드 음이온으로 환원시킨 후 요오드 음이온 측정법과 동일하게 수행하였다. 이 방법은 검출한계가 해수에서 0.1 ng/ml이었으며 검량선은 0.9997의 좋은 상관계수값을 보였다. 이 방법은 또한 재현성이 우수하고 간단하여 해수에 인체의 필수원소인 요오드를 낮은 농도까지 분석하는데 유용하게 사용될 수 있다고 사료된다.

• Environmental Analysis Health and Toxicology
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• 제17권1호
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• pp.37-51
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• 2002

Eleven phenols including two chlorophenols, eight alkylphenols and bisphenol A were derivatized with isobutylchloroformate to form their isobutoxycarbonyl derivatives. Standard phenol mixture was concentrated for the isobutoxycarbonyl (isoBOC) derivatization and analysed by gas chromatography/mass spectrometry (GC/MS). The recoveries of the derivatization method of alkylphenols, chlorophenols, and bisphenol A were calculated by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison; shaking and heating method. The linear detector responses were obtained in the concentration range of 5∼400 ng, with correlation coefficients varying from 0.9755∼0.9981. Recoveries of the alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode using two work-up methods for comparison ; the US-EPA method and the isoBOC derivatization method, Eleven phenols in water samples were extracted with dichloromethane and then concentrated. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 85.1∼109.9％ and 90.3∼126.6％ for the US-EPA method and the isoBOC.

• 분석과학
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• 제13권5호
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• pp.592-600
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• 2000

담즙내 지방산의 농도와 그 조성이 콜레스테롤의 과포화와 마찬가지로 담석 형성 과정에 관련이 있는 것으로 여겨지고 있다. 본 연구에서는 gas chromatography-mass spectrometry (GC-MS)의 selected ion monitoring (SIM) 방법을 이용하여 담즙내 23종의 지방산 동시 분석을 시도하였다. 전처리 과정의 첫 단계로 유리 지방산과 인지질 지방산을 분리하기 위해 aminopropyl column을 사용하였고 GC-MS에서의 검출을 위하여 유리 지방산은 MSTFA/TMCS 혼합액으로 유도제화를 실시하였으며 인지질 지방산의 경우는 염기를 이용한 가수분해를 실시한 뒤 위와 동일한 과정으로 유도제화하였다. 이 때의 회수율은 61.1-99.0% 이었으며 각각 3.1-25.6%와 3.8-27.0%의 within-a-day와 day-to-day 분석의 RSD 값을 얻었다. 이 방법을 적용하여 정상인과 담석증 환자의 담즙내에 존재하는 유리 및 인지질 지방산의 농도를 알아보았으며 이 때 각 물질들의 농도와 분포가 두 군간에 차이를 나타냄을 알 수 있었다.

• 분석과학
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• 제13권5호
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• pp.666-674
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• 2000

본 연구는 기체크로마토그래피-질량분석법을 이용한 생물시료 중 polybrominated biphenyls(PBBs)의 분석법을 설명하였다. 생물 시료 중 PBB류는 40mL 아세톤과 80mL의 헥산 혼합용매에서 초음파추출기 20분간 교반하여 추출하였다. 추출액 중 존재하는 지질성분은 농축 황산용액으로 분해한 후 PBB류는 Florisil 컬럼으로 정제하였다. PBB류를 정량분석하기 위하여 정제액은 GC/MS-selected ion monitoring 방법에 의해 분석하였다. 본 실험 조건하에서 전반적인 PBB류의 추출율은 77-111%로 나타났다.

• Bulletin of the Korean Chemical Society
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• 제32권3호
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• pp.977-980
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• 2011

A new analytical method for measurement of 3,4-dihydroxyphenylalanine (DOPA) in human urine was developed. DOPA from an aqueous solution was converted into an ethoxycarbonyl (EOC) derivative. A tertbutyldimethylsilyl (TBDMS) reaction under anhydrous conditions was then attempted for analysis by gas chromatography-mass spectrometry in selected ion monitoring mode. A new mass spectral data on DOPA as a tri-EOC/mono-TBDMS derivative was built. This method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.1-9.2), and accuracy (% relative error = -7.2-8.8), with a detection limit of 0.05 ng/mL. This selective and accurate method of DOPA analysis will be useful for biochemical monitoring of various neurological disorders including Parkinson's disease in biological fluids.

• 한국축산식품학회지
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• 제29권4호
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• pp.482-486
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• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• 한국식품위생안전성학회지
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• 제8권1호
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• pp.17-23
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• 1993

In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.