• 분석과학
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• 제14권2호
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• pp.180-190
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• 2001

화합물에 포함된 냄새를 유발하는 물질은 다양한 성분으로 되어 있다. 냄새를 유발하는 휘발성 화합물의 분석에는 GC 또는 GC/MSD 등이 많이 사용된다. 그러나, 이들 분석기기는 전체 휘발성 성분의 profile이나 특정성분의 함량을 정량적으로 분석할 수는 있으나, 냄새를 유발하는 지배적인 성분이 무엇인지 파악하기가 어렵다. 이러한 문제점을 해결하기 위해 사용되는 방법에는 GC-Sniffing 또는 GC-Olfactometry법 등이 있다. 본 연구에서는 복합적인 냄새성분을 검출하기 위해 사람의 후각을 이용하는 olfactometry를 기존 GC에 결합시켜 분리컬럼에서 분리된 시료가 동시에 검출되는 GC/FID/Olfactometry를 개발하였다. FID와 ODP 신호간의 시간차이는 물질의 종류와 농도, 그리고 패널에 따라 다르게 나타났다. 일반적으로 휘발성과 냄새강도는 큰 물질일수록, 패널의 호흡주기가 짧을수록 두 신호간의 시간차이가 적었다. 그러므로, 정확한 냄새 원인물질의 규명에는 이들 신호의 관계에 대한 고찰이 필요하다.

• 한국산업보건학회지
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• 제16권3호
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• pp.222-232
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• 2006

Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

• 환경위생공학
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• 제17권2호
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• pp.34-39
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• 2002

This study was performed to survey and evaluate the contents of di-n-butyl phthalate(DBP) in manicures by GC/FID and GC/MSD. The tested samples were 61 domestic and 41 imported manicures circulating in Seoul and Kyonggi-Do area. DBP was detected respectively in the rate of 93.4% for domestic manicures and 43.9% for imported manicures. The contents of DBP in domestic and imported manicures were 11.6g/17g~74.7g/kg and 28.2g/kg~78.9g/kg respectively. DBP was used in domestic and imported manicures with the exception of Japan products. Therefore, the alternative material for DBP should be developed and used to ensure consumers' safety.

• 한국대기환경학회지
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• 제15권2호
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• pp.121-138
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• 1999

This study was carried out to evaluate the performance of a sampling and analytical methodology for the measurement of selected volatile organic compounds (VOCs) in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/FID and GC/MSD analysis. Target analytes were aromatic VOCs, including BTEX, 1,3,5-and 1,2,4,-trimethylbenzenes(TMBs), and naphthalene. The methodology was investigatedwith a wide range of performance criteria such as repeatability, linearity, lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal and external standards. standards. Stability of samples collected on adsorbent tubes during storage was also investigated. In addition, the sampling and analytical method developed during this study was applied to real samples duplicately collected in various indoor and outdoor environments. Precisions for the duplicate samples and distributed volume samples appeared to be well comparable with the performance criteria recommended by USEPA TO-17. The audit accuracy was estimated by inter-lab comparison of both duplicate samples and standard materials between the two independent labs. The overall precision and accuracy of the method were estimated to be within 30% for major aromatic VOCs such as BTEX. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

• 한국식품영양과학회지
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• 제31권6호
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• pp.953-957
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• 2002

새우를 육과 껍질 부분을 분리하지 않는 것과 폐기되고 있는 껍질부분만을 모아 SDE 장치를 이용해서 휘발성 성분을 조사해 본 결과, 각각 26개와 46개의 성분이 분리된 것을 알수 있었다. 휘발성 성분의 양에서도 껍질 부분을 처리한 시료에서 훨씬 더 많은 것을 볼 수 있었다. 시료를 마쇄하는 전처리 공정을 거치면서 추출율을 살펴보면 SSW의 경우에는 눈에 띄게 휘발성 성분의 양이 늘어난 것을 알 수가 있었다.. GC-MSD로 분리.동정 한 결과, pyrazines이 9종, acids S종, aldehydes 3종, alcohol 4종, pyridines 2종로 나타났다. SSW를 AEDA법으로 단계적으로 희석하여 GCO를 통해 sniffing test를 실시한 결과, 낮은 온도에서는 진한 새우 새우냄새가 지배적이었고, 온도가 올라갈수록 불쾌한 기름 냄새가 났다. GC-FID에서는 검출되지 않는 영역에서도 고소한 향이나 부드러운 향성분이 log$_3$ FD3이상의 높은 향 인지도를 나타내었다.

• 농약과학회지
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• 제8권2호
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• pp.129-136
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• 2004

생장조절제 Atonic 원제 중 부성분의 함량과 화학구조를 구명하기 위하여 diethyl ether와 dichloromethane 분배액을 각각 GC-FID와 GC-MSD로 분석하여 5종 부성분의 화학구조를 구명하였다. 주성분인 Atonic의 함량은 약 84%이었으며, 부성분의 함량은 $0.24\sim10.74%$이었다. 확인된 부성분은 2-methoxy-phenol (guaiacol, m/z 124), 2-chloro-6-methoxyphenol 또는 4-chloro-6-methoxyphenol (m/z 158), 1,2-dimethoxy-4-nitrobenzene (m/z 183), 그리고 2,6-bis(1,1-dimethylethyl)-4-methylphenol (m/z 220)이었으며, 국내에서 규제중인 6종의 유해성분은 포함되지 않은 것으로 판단되었다.

• 분석과학
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• 제31권1호
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• pp.23-30
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• 2018

어린이 제품 중 22 종의 알러지 유발 방향성 물질들을 기체 크로마토그래피 불꽃 이온화 검출기(GC-FID)와 기체 크로마토그래피 질량 분석기(GC-MSD)를 사용하여 분석하였다. 분석물질들은 자동속슬렛 추출장치를 사용하여 추출하였으며, 고속 냉동 원심분리기에서 10분동안 원심분리 후 상징액을 2 mL vial 옮겨 Split mode로 주입하여 분석하였다. 확립된 조건에서 검정곡선은 0.996 이상의 상관계수를 갖는 직선성을 보였으며, 감도의 경우는 6.7~1,859,839로서 물질별로 기기특성 및 검출기에 따라 상당히 넓은 범위의 감도를 나타내었다. 기기검출한계는 $0.0032{\sim}0.0335{\mu}g/mL$로서 최대 약 $0.1{\mu}g/mL$이하의 기기검출한계를 나타내었고, 방법검출한계는 $0.0033{\sim}0.1161{\mu}g/mL$의 범위를 나타내었다. 또한 정량한계는 $0.0100{\sim}0.5422{\mu}g/mL$의 범위를 보였고, 정밀도는 0.21~4.89 %, 정확도는 89~111%의 범위를 나타내었다. 본 연구에서 개발한 분석법으로 시판품에 실제 적용하였다.

• 한국식품과학회지
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• 제32권1호
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• pp.56-61
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• 2000

청갓으로 만든 갓김치의 휘발성 화합물의 종류를 GC/FID와 GC/MSD를 사용하여 분리 동정하고, 발효 숙성 중 isothiocyanates와 그 유도체함량의 변화를 측정하였다. 청갓 김치의 수증기 증류물로부터 14종의 휘발성화합물을 분리, 동정하였으며 그 중 hexadecanoic acid를 비롯한 acid와 nitromethane등의 hydrocarbons류가 전체의 63%이상을 차지하였다. 갓의 특징적인 자극성 성분으로 알려진 isothiocyanates와 유도체들의 함량은 전체화합물의 30%로, 2-phenylethyl isothiocyanate가 주요성분이었고, 그밖에 benzothiazole 2-methylbenzothiazole, 2-(3H)-benzothiazolone 등이 동정되었다. 청갓 김치의 발효숙성 중 isothiocyanates와 그 유도체들의 상대적 함량 변화는 저장4일 이후부터 뚜렷하게 감소되었으며, 그 중 2-phenylethyl isothiocyanate경우 저장 7일째에 50%이상, 저장 14일째에는 80%이상 소실되는 것으로 나타났다.

• 한국연초학회지
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• 제27권1호
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• pp.100-106
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• 2005

To obtain the optimum condition for analysis of 10 alkaloids in tobacco leaves, such as nicotine, nornicotine, anatabine, anabasine, myosmine, cotinine, 2,3'-dipyridyl, $\beta-nicotyrine,\;\beta-nornicotyrine\;and\;\beta-formylnornicotin$, 5 types of extraction method were investigated by GC-FID and GC/MS. The optimum condition of alkaloid extraction was achieved by using methanol:dichloromethane(1:3, v/v) after NaOH treatment. The use of mass selective detector (MSD) provided unambiguous nicotine related alkaloid analysis. Alkaloids in various tobacco leaves were extracted with the optimum extraction condition and quantified by GC/MS/SIM mode. Compared with concentrations of alkaloids among the various tobacco leaves, the concentration of alkaloids was generally in the order burley > flue-cured > oriental tobacco. In flue-cured tobacco leaves, the order of concentration of alkaloids was nicotine > anatabine > nornicotine > $\beta-nicotyrine\;>\;\beta-formylnornicotine\; >\;myosmine\;>\;2,3'-dipyridyl\;>\;cotinine\;>\;anabasine\;>\;\beta-nornicotyrine$. However, in the case of burley and oriental tobacco leaves, the concentration of nornicotine was higher than that of anatabine.

• 한국식품영양학회지
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• 제13권2호
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• pp.118-124
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• 2000

Lipoxygenase(LOX) in soybeans is responsible for beany flavors which limit the wide utilization of soybeans to foods. This study was conducted to analyze beany flavor compounds of the normal Hwagkeumkong and LOX-deficient soybean cultivars, Jinpumkong which lacks L-2, L-3, and Jinpumkong 2 which lacks all L-1, L-2, L-3. Using the combination of dynamic headspace sampling and gas chromatography-mass selective detector(DHS-GC-MSD) for analyzing volatile compounds, hexanal and hexanol were identified in whole soy flour of all three soybena cultivars. Hwangkeumkong had more volatile compounds than Jinpumkong and Jinpumkong 2 in defatted soy flour. Hexanal and acetic acid were identified in soy milk of all three soybean cultivars but Hwangkeumkong had more volatile compounds than Jinpumkong 2. From the analysis with a static headspace sampling(SHS) and GC-MSD the major compounds were hexanal, acetic acid, 1-hexanol, and 1-octen-3-ol. The content of acetic acid was similar among three cultivars. But contents of hexanal and pentanal in Jinpumkong 2 were less than that of Jinpumkong and Hwangkeumkong. Using GC-FID, Jinpumkong 2 had less contents of hexanal and pentanol than Hwangkeumkong in whole soy flour and defatted soy flour. In this study, LOX-deficient soybean cultivars showed less hexanal, pentanol and other compounds than the normal Hwangkeumkong. However quite amount of beany flavor compounds were identified in Jinpumkong and Jinpumkong 2. So further studies are required to characterize LOX isozymes, to understand the mechanisms of beany flavors production, and to develop some other methods for removing beany flavor.