Identification of nitroaromatics in diesel exhaust particulate using gas chromatography/negative ion chemical ionization mass spectrometry and other techniques

Newton, David L.; Erickson, Mitchell D.; Tomer, Kenneth B.; Pellizzari, Edo D.; Gentry, Pamela.; Zweidinger, Roy B.

doi:10.1021/es00098a007

Cited by 87 publications

(30 citation statements)

References 16 publications

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“…For diesel vehicle exhaust, as reported before, nitro-PAHs contribute to a varying degree to the mutagenicity (14)(15)(16). In this investigation, the distribution pattern of the mutagenic activity is similar for the three samples, although an enhanced activity could be seen in subfraction 2A of the diesel extract.…”

Section: Subfraction Iv:3supporting

confidence: 81%

Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

Strandell

Zakrisson

Alsberg

et al. 1994

Environ Health Perspect

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SwedenExtracts of gasoline and diesel vehicle exhaust and ambient air particles were fractionated into five fractions according to polarity on a silica gel column. Two medium polar fractions showing high genotoxic activity in the Ames test were further subfractionated, using normal-phase high-performance liquid chromatography. Chemical analyses were performed by means of gas chromatography combined with mass spectrometry and flame ionization and detection. The crude extracts, fractions, and subfractions were assayed with the Ames test, with and without S9, and the most abundant compounds in the subfractions are reported. -Environ Health Perspect 1 02(Suppl 4): 85-92 (1994).

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Section: Subfraction Iv:3supporting

confidence: 81%

Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

Strandell

Zakrisson

Alsberg

et al. 1994

Environ Health Perspect

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“…7 The analytical measurement of nitro-PAH has been addressed by several chromatographic methods. High performance liquid chromatography (HPLC) with both UV and electrochemical detection, 8 and the capillary gas chromatography (CGC) with flame ionization, 8,9 electron capture, 9 nitrogen and phosphorus, 9,10 and mass spectrometry [11][12][13][14] detection were largely used for determination of nitro-PAH in atmosphere or airparticulates. 15 However, no analytical methods have been established for detection of this compound class in water, neither capillary liquid chromatography (μLC) has been evaluated, 16 thus encouraging us to conduct the present work.…”

Section: Introductionmentioning

confidence: 99%

Solid-phase extraction of nitro-PAH from aquatic samples and its separation by reverse-phase capillary liquid chromatography

Toledo¹,

Lanças²,

Carrilho³

2007

J. Braz. Chem. Soc.

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Neste trabalho é proposta uma metodologia analítica para extrair 1-nitronaftaleno, 2-nitrofluoreno, 9-nitroantraceno, 3-nitrofluoranteno e 1-nitropireno como compostos modelos para nitropoliaromáticos (nitro-HPA) em amostras aquáticas. A cromatografia líquida capilar com detecção UV on-column (μLC-UV) foi empregada para separar e quantificar todos os cinco nitro-HPA extraídos. Duas técnicas diferentes de extração foram testadas e comparadas: extração líquido-líquido (LLE) e extração em fase sólida (SPE) com dois diferentes tipos de sorbentes: partículas octadecilssilica (C 18 ) e estireno divinilbenzeno (XAD-2). A eluição dos analitos foi testada com diclorometano e acetonitrila. O melhor resultado de recuperação foi obtido para extração SPE -C 18 com diclorometano com valores variando de 76 a 97% e valores de desvio padrão relativo menores que 4%. As condições cromatográficas para análise foram desenvolvidas empregando uma coluna capilar (250 × 0,3 mm) empacotada com partículas C 18 de 5 μm com eluição isocrática de 65% de acetonitrila em água (v/v) com vazão de 7 μL min -1 . Os limites de detecção obtidos no sistema UV on-column (abrangendo de ~3 a 30 μmol L -1 ) são limitantes para uma aplicação ambiental, porém adequados a estudos de toxicidade.In this work, an analytical methodology to extract 1-nitronaphthalene, 2-nitrofluorene, 9-nitroanthracene, 3-nitrofluoranthene, and 1-nitropyrene aquatic samples is proposed. Capillary liquid chromatography with on-column UV detection (μLC-UV) was employed to separate and quantitate all five nitrated polycyclic aromatic hydrocarbons (nitro-PAH) extracted from water samples. Two different extraction techniques were tested and compared: liquid-liquid extraction (LLE) and solid phase extraction (SPE) with two different sorbents, octadecylsilica (C 18 ) and styrene divinylbenzene (XAD-2) particles. The elution of analytes was tested with both acetonitrile and methylene chloride. The best recovery results were obtained for SPE-C 18 extraction with the methylene chloride with values ranging from 76 to 97% with RSD values smaller than 4%. The chromatographic conditions for analysis was carried out using a 250 × 0.3 μm i.d. packed capillary column with 5 μm C 18 particles. The elution was isocratic with 65% acetonitrile in water (v/v) as mobile phase with a flow rate of 7 μL min -1. The detection limits due to on-column UV detection (ranging ~3 -30 μmol L -1 ) are limiting for environmental applications, however, they are suited for toxicological studies.

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“…Nitro-PAHs in the environment are formed primarily as a result of reactions between PAHs and nitrogen oxides and/or nitric acid, all of which are commonly found in combustion effluents [7,8,9]. Diesel engines, in particular, have been a major source of nitro-PAHs [9,10]. Typically nitro-PAHs are found at low µg g -1 concentration levels in complex environmental matrices; therefore, analytical methods used for the measurement of nitro-PAHs must exhibit both high selectivity and sensitivity.…”

Section: Introductionmentioning

confidence: 99%

Determination of nitrated polycyclic aromatic hydrocarbons in diesel particulate-related standard reference materials by using gas chromatography/mass spectrometry with negative ion chemical ionization

et al. 2003

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Gas chromatography/mass spectrometry (GC/MS) with negative ion chemical ionization (NICI) detection was utilized for quantitative determination of nitrated polycyclic aromatic hydrocarbons (nitro-PAHs) in diesel particulate-related standard reference materials (SRMs). Prior to GC/MS analysis, isolation of the nitro-PAHs from the complex diesel particulate extract was accomplished using solid phase extraction (SPE) and normal-phase liquid chromatographic (LC) fractionation using an amino/cyano stationary phase. Concentrations of eight to ten mononitro-PAHs and three dinitropyrenes were determined in three diesel particulate-related SRMs: SRM 1650a Diesel Particulate Matter, SRM 1975 Diesel Particulate Extract, and SRM 2975 Diesel Particulate Matter (Industrial Forklift). The results from GC/MS NICI using two different columns (5% phenyl methylpolysiloxane and 50% phenyl methylpolysiloxane) were compared to each other and to results from two other laboratories for selected nitro-PAHs. 1-Nitropyrene was the most abundant nitro-PAHs in each of the diesel particulate SRMs (19.8+/-1.1 micro g g(-1) particle in SRM 1650a and 33.1+/-0.6 micro g g(-1) particle in SRM 2975). Three dinitropyrene isomers were measured in SRM 1975 at 0.5-1.4 micro g g(-1) extract and in SRM 2975 at 1-3 micro g g(-1) particle.

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Identification of nitroaromatics in diesel exhaust particulate using gas chromatography/negative ion chemical ionization mass spectrometry and other techniques

Cited by 87 publications

References 16 publications

Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

Chemical analysis and biological testing of a polar fraction of ambient air, diesel engine, and gasoline engine particulate extracts.

Solid-phase extraction of nitro-PAH from aquatic samples and its separation by reverse-phase capillary liquid chromatography

Determination of nitrated polycyclic aromatic hydrocarbons in diesel particulate-related standard reference materials by using gas chromatography/mass spectrometry with negative ion chemical ionization

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