• Mass Spectrometry Letters
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• 제4권1호
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• pp.18-20
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• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• 분석과학
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• 제12권4호
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• pp.265-272
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• 1999

에스트로겐처럼 행동하여 호르몬 수용체와 결합하거나 세포의 신호전달 과정에 영향을 미침으로서 내분비계를 교란시킬 수 있는 환경 에스트로겐 19종 (phytoestrogen: 12종, mycoestrogen: 5종, synthetic estrogen: 2종)의 동시 프로필 분석을 시도하였다. Gas Chromatography/Mass Spectrometry (GC/MS)의 selected ion monitoring (SIM) 방법을 기본으로 하였으며, 액체-고체 추출, 효소 기수분해, 액체-액체 추출 그리고 trimethylsilyl (TMS)-ether 형태의 유도체화를 거치는 비교적 간편한 전처리 방법으로 47.6~99.5%의 회수율과 0.66~9.33%, 1.66~16.14%의 within-a-day 및 day-to-day 분석의 RSD 값을 얻었다. 이 방법을 적용하여 정상 성인 여성과 남성의 뇨 시료에 존재하는 대상 물질들의 농도범위를 결정함으로서 환경 에스트로겐의 영향을 평가하는데 기준이 될 수 있는 한국인 정상인 참고치를 설정하였다.

• Environmental Engineering Research
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• 제23권4호
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• pp.390-396
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• 2018

This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

• Mass Spectrometry Letters
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• 제11권4호
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• pp.103-107
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• 2020

We report the application of 2,4,6-trichlorobenzoyl chloride (often referred to as Yamaguchi esterification reagent) for the selective derivatization of the carboxylic group for GC-MS with the sample preparation method optimized for GC-MS analysis. The reagent was shown to be capable of selectively turning the carboxylic group into a reaction center, i.e., anhydride, of which the further reaction was directed to a near complete formation of required esters by unique steric and electronic effects of the reagent. Using the developed method, the chiral separation of hydroxycarboxylic acids by GC-MS using non-chiral columns was successfully demonstrated.

• Mass Spectrometry Letters
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• 제12권2호
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

• Mass Spectrometry Letters
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• 제4권4호
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• pp.75-78
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• 2013

A gas chromatography/mass spectrometric (GC/MS) method was developed as a candidate reference method for the accurate determination of essential fatty acids (linoleic acid, ${\alpha}$- and ${\gamma}$-linolenic acids) in food supplemental oil products. Samples were spiked with three internal standards (stearic acid-$d_{35}$, $^{13}C_{18}$-linoleic acid, and $^{13}C_{18}$-${\alpha}$-linolenic acid). Samples were then subject to saponification, derivatization for methylation, and extraction by organic solvent. For GC/MS measurement, an Agilent HP-88 column, designed for the separation of fatty acid methyl esters, was selected after comparing with other columns as it provided better separation for target analytes. Target analytes and internal standards were detected by selected ion monitoring of molecular ions of their methyl ester forms. The GC/MS method was applied for the measurement of three botanical oils in NIST SRM 3274 (borage oil, evening primrose oil, and flax oil), and measurement results agreed with the certified values. Measurement results for target analytes which have corresponding isotope-labeled analogues as internal standard were calculated based on isotope dilution mass spectrometry (IDMS) approach, and compared with results calculated by using the other two internal standards. Results from the IDMS approach and the typical internal standard approach were in good agreement within their measurement uncertainties. It proves that the developed GC/MS method can provide similar metrological quality with IDMS methods for the measurement of fatty acids in natural oil samples if a proper fatty acid is used as an internal standard.

• 한국식품위생안전성학회지
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• 제12권3호
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• pp.210-216
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• 1997

The prevention of oxidative degradation in fats and oils is largely controlled by the use of synthetic phenolic antioxidants. Antioxidants, BHA: 2-&-3-tert-butyl-4-hydroxyanisol, BHT: 3,5-di-tert-butyl-4-hydroxytoluene, TBHQ: tert-butylhydroquinone, PG: propyl gallate, PTG: pentyl gallate, OG:octyl gallate, were extracted from fatty foods with hexane and from hexane layer to presaturated acetonitrile with hexane. The polar phenolic hydroxyl groups of antioxidants were silylated with MSTFA and injected to Gas Chromatography/Mass Spectrometry. The calibration plots were linear in the investigated range, 0.1~10.0 $\mu\textrm{g}$/g. The limit of detection for 6 phenolic antioxidants was 0.1 $\mu\textrm{g}$/g. Recoveries and reproducibilities from samples fortified at 1.0 $\mu\textrm{g}$/g were in the range of 70~90% and 0.5~13%, respectively. The simultaneous determination of phenolic antioxidants in fatty foods using GC/MS-SIM mode and macro program was described.

• 한국식품위생안전성학회지
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• 제8권1호
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• pp.9-15
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• 1993

어패류를 포함한 식용 육류중에 잔류하는 항생물질 및 항균성물질을 검출하기 위하여, 분석기기로서 Gas chromatography/ Mass spectrometry(GC/MS)를 사용한 동시분석법을 개발하였다. 여러 항생.항균제중에서 penicillin G, chloramphenicol, thiamphenicol을 중심으로 간단한 전처리과정과 유도체화를 하여 GC/MS 분석을 시행하였다. 전처리 과정을 요약하면 pH 4.0의 0.01 M EDTA-2Na McIlvaine buffer로의 추출, n-hexane으로의 탈지, Bond-Elute $C_{18}$ cartridge에 흡착된 물질의 0.01 M-methnolic oxalic acid로의 용출 그리고 건조 후 유도체화의 순으로 되어 있다. 본 방법에 의한 1 ppm spike시의 회수율은 penicillin G, chloramphenicol, thiamphenicol 각각 63.5%, 76.3%, 84.7%이었고, 검출한계는 각각 시료 g당 0.6, 0.085, $0.084\;\mu\textrm{g}$이었다. 또한 GC/MS 확인과정에서 실제 잔류농도가 1 ppm 이상이면 full scan spectrum으로 확인이 가능하였다. 이와 같은 GC/MS에 의한 잔류물질의 정량 및 확인시험은 앞의 미생물학적 방법의 복원은 물론 식품의 안전성 재고 및 규제독성의 측면에서도 매우 뜻 있는 연구라 하겠다.

• 분석과학
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• 제14권2호
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• pp.109-114
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• 2001

담배에 포함된 향료 성분을 headspace solid phase microextraction(SPME)를 이용하여 gas chromatography-mass spectrometry(GC-MS)의 selected ion monitoring(SIM)방법으로 분석하였다. 본 연구에서 사용한 담배향과 관련된 성분은 estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methylisoeugenol 및 myristicin 등 11종이며 분석결과 모든 담배에서 한가지 또는 그 이상의 담배향 성분을 $0.001-1.3{\mu}g/g$ 검출할 수 있었으며 회수율은 89.1-102.9%로 나타났고 상대표준편차는 2.6-25.2%를 얻었다.

• Preventive Nutrition and Food Science
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• 제16권1호
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• pp.45-54
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• 2011

Volatile components in commercial pine needle (Pinus densiflora S. and Z.) powder were extracted using simultaneous steam distillation and a solvent extraction (SDE) apparatus, and were analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 230 compounds divided into 13 groups were identified, which included alcohols (42), ketones (39), aldehydes (32), terpenes (30), alkenes (17), esters (14), furans (14), benzenes (10), alkanes (8), napthalenes (7), acids (6), miscellaneous compounds (6), and phenols (5). Among the 230 compounds identified, 96 compounds were positively confirmed and quantified, and the rest of the compounds were tentatively identified. The major volatile components identified at relatively high levels were dodecanoic acid, hexadecanoic acid, hexanal, benzaldehyde, (Z)-3-hexen-1-ol, 1-penten-3-one, limonene, and $\beta$-caryophyllene oxide. Among the groups, terpenes accounted for 60.18% of the total concentration of all the volatile components. Some volatile components might account for the unique aroma and the biological activity of the sample.