• Asian Journal of Atmospheric Environment
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• 제11권4호
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• pp.283-299
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• 2017

An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

• 한국대기환경학회지
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• 제34권1호
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• pp.120-143
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• 2018

The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

• Asian Journal of Atmospheric Environment
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• 제4권1호
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• pp.1-8
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• 2010

The effectiveness of the government regulation on tail-pipe emission for diesel vehicles issued in 2003 in Tokyo was evaluated in this study. Variations in annual average concentrations of polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs associated with airborne particulate matter were investigated in connection with the variation in airborne elemental carbon (EC) concentration in downtown Tokyo, Japan in 2006-2007 and in 1997-1998. The annual average concentrations of EC, seven different PAHs, and 1-nitropyrene were found to have decreased significantly from 1997-1998 to 2006-2007. The most prominent decrease in atmospheric concentration was observed for 1-nitropyrene, which is a representative nitro-PAH originating from diesel vehicles. This indicated that the government control has worked to considerably reduce both atmospheric mutagens and airborne particulate matter. In contrast, the concentrations of two nitro-PAHs, 2-nitrofluoranthene and 2-nitropyrene, remained the same. These nitro-PAHs are known to be formed by atmospheric nitration of their parent PAHs, and this result suggested factors other than the concentration of parent PAHs and $NO_2$ affects the degree of atmospheric formation of nitro-PAHs.

• 분석과학
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• 제10권5호
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• pp.315-324
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• 1997

Benzo(a)pyrene을 비롯한 16종의 polycyclic aromatic hydrocarbon(PAHs)과 4종의 nitro-PAHs를 reversed-phase liquid chromatography/diode array detection (RPLC/DAD)를 이용하여 기울기용리법으로 분리하고, PAH류의 머무름거동에 영향을 미치는 인자들, 즉 탄소수, F인자, L/B ratio, 물에 대한 용해도 및 방해수소원자쌍의 수와 시료의 머무름과의 상관관계를 고찰하였다. 대부분의 PAH류는 탄소원자수와 F값이 커질수록 logk'이 증가하는 사실을 확인하였다. 그리고 몇 가지 이성체들과 nitro-PAH류들은 용해도가 크고, L/B값이 작으며, 방해수소원자쌍의 수가 많을수록 먼저 용리됨을 확인하였다. 각 PAH류의 검출한계는 100~500ng/mL 범위로 나타났으며, 실제 물시료에 대한 검출한계(method detection limit, MDL)는 0.1~0.5ng/mL 범위였다.

• 대한약학회:학술대회논문집
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• 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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• pp.284.1-284.1
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• 2002

In previous studies, we demonstrated that ambient PM collected from urban site of Korea air could induce DNA damage, Various mutagens and carcinogens present in the urban air differ according to the source of the pollutants. Polycyclic aromatic hydrocarbons (PAHs) and their nitrated compound are produced in the combustion of fossil fuels as diesel emission exhausts. In recent, PAH and nitro-PAH have been identified in urban air particulate matter (PM). and some of them were found to be tumorigenic in experimental animals and humans. (omitted)