GC/MS Analysis of European Union (EU) Priority Polycyclic Aromatic Hydrocarbons (PAHs) using an Agilent J&W DB-EUPAH GC Column with a Column Performance Comparison
Applications | 2010 | Agilent TechnologiesInstrumentation
Polycyclic aromatic hydrocarbons (PAHs) represent a class of toxic environmental contaminants with recognized carcinogenic and mutagenic properties. Regulatory bodies in the European Union have established a list of 15 priority PAHs plus an additional marker compound to ensure food safety. Accurate separation and quantitation of these isomeric analytes remain challenging on conventional nonpolar gas chromatography (GC) columns, particularly for critical pairs and high–molecular weight dibenzopyrene isomers.
This study aimed to develop and validate a GC/MS method for the determination of the EU 15+1 priority PAHs using an Agilent J&W DB-EUPAH capillary column. A performance comparison versus a commonly used Restek Rxi-17 column was conducted to assess chromatographic resolution, sensitivity, bleed characteristics, and quantitation reliability for all target analytes.
Standard mixtures containing the 15+1 EU PAHs were prepared at concentrations ranging from 0.1 to 10 µg/mL in acetone. A 0.5 µL splitless injection was performed on an Agilent 6890N GC coupled to a 5975B MSD, using helium as the carrier gas. The oven program ramped from an initial 45 °C hold through multiple temperature ramps up to 320 °C. Three critical isomeric pairs and four dibenzopyrene isomers were monitored and resolution factors calculated to evaluate separation efficiency.
The DB-EUPAH column achieved baseline resolution for all 16 target PAHs within 43 minutes, including three challenging isomeric pairs with resolution factors (Rs) exceeding 1.6. Critical separation of benzo[j]fluoranthene from its [b] and [k] isomers (Rs ≥ 1.6) and of indeno[1,2,3-cd]pyrene from dibenz[a,h]anthracene (Rs ≈ 2.6) enabled individual quantitation. In a direct column comparison at 320 °C, the DB-EUPAH exhibited significantly lower bleed, resulting in twofold higher signal-to-noise ratios for late-eluting dibenzopyrene isomers relative to the Rxi-17 column. The improved peak shapes and sensitivity on DB-EUPAH translated into lower detection limits and more reliable trace-level analysis.
Advances in low-thermal-mass GC systems, rapid temperature programming, and integrated backflush capabilities are expected to further reduce analysis time and increase throughput. Development of even more selective midpolar phases and coupling with high-resolution mass spectrometry will enhance specificity for complex matrices. Automation of sample preparation and data processing will streamline routine monitoring of PAHs in food and environmental samples.
The Agilent J&W DB-EUPAH column delivers superior separation and sensitivity for the EU 15+1 priority PAHs compared to a conventional Rxi-17 phase. Its low bleed at high temperatures and strong chromatographic performance make it a robust choice for trace-level GC/MS analysis of complex PAH mixtures.
GC/MSD, GC/SQ, GC columns, Consumables
IndustriesEnvironmental
ManufacturerAgilent Technologies
Summary
Significance of the Topic
Polycyclic aromatic hydrocarbons (PAHs) represent a class of toxic environmental contaminants with recognized carcinogenic and mutagenic properties. Regulatory bodies in the European Union have established a list of 15 priority PAHs plus an additional marker compound to ensure food safety. Accurate separation and quantitation of these isomeric analytes remain challenging on conventional nonpolar gas chromatography (GC) columns, particularly for critical pairs and high–molecular weight dibenzopyrene isomers.
Objectives and Study Overview
This study aimed to develop and validate a GC/MS method for the determination of the EU 15+1 priority PAHs using an Agilent J&W DB-EUPAH capillary column. A performance comparison versus a commonly used Restek Rxi-17 column was conducted to assess chromatographic resolution, sensitivity, bleed characteristics, and quantitation reliability for all target analytes.
Methodology
Standard mixtures containing the 15+1 EU PAHs were prepared at concentrations ranging from 0.1 to 10 µg/mL in acetone. A 0.5 µL splitless injection was performed on an Agilent 6890N GC coupled to a 5975B MSD, using helium as the carrier gas. The oven program ramped from an initial 45 °C hold through multiple temperature ramps up to 320 °C. Three critical isomeric pairs and four dibenzopyrene isomers were monitored and resolution factors calculated to evaluate separation efficiency.
Instrumentation
- Agilent 6890N Network GC with 7683B autosampler
- Agilent 5975B mass spectrometer (electron ionization, scan 50–550 amu)
- Agilent J&W DB-EUPAH column (20 m × 0.18 mm id, 0.14 µm film)
- Restek Rxi-17 column (20 m × 0.18 mm id, 0.18 µm film) for comparison
- Helium carrier gas, splitless inlet at 325 °C
Main Results and Discussion
The DB-EUPAH column achieved baseline resolution for all 16 target PAHs within 43 minutes, including three challenging isomeric pairs with resolution factors (Rs) exceeding 1.6. Critical separation of benzo[j]fluoranthene from its [b] and [k] isomers (Rs ≥ 1.6) and of indeno[1,2,3-cd]pyrene from dibenz[a,h]anthracene (Rs ≈ 2.6) enabled individual quantitation. In a direct column comparison at 320 °C, the DB-EUPAH exhibited significantly lower bleed, resulting in twofold higher signal-to-noise ratios for late-eluting dibenzopyrene isomers relative to the Rxi-17 column. The improved peak shapes and sensitivity on DB-EUPAH translated into lower detection limits and more reliable trace-level analysis.
Benefits and Practical Applications
- Accurate quantitation of EU 15+1 PAHs in food safety and environmental monitoring
- Enhanced resolution of isomeric and high-molecular weight PAHs
- Improved sensitivity and lower detection limits for heavy dibenzopyrenes
- Reduced column bleed at elevated temperatures, extending method robustness
Future Trends and Applications
Advances in low-thermal-mass GC systems, rapid temperature programming, and integrated backflush capabilities are expected to further reduce analysis time and increase throughput. Development of even more selective midpolar phases and coupling with high-resolution mass spectrometry will enhance specificity for complex matrices. Automation of sample preparation and data processing will streamline routine monitoring of PAHs in food and environmental samples.
Conclusion
The Agilent J&W DB-EUPAH column delivers superior separation and sensitivity for the EU 15+1 priority PAHs compared to a conventional Rxi-17 phase. Its low bleed at high temperatures and strong chromatographic performance make it a robust choice for trace-level GC/MS analysis of complex PAH mixtures.
References
- P. Mottier, V. Parisod, R. J. Turesky, J. Agric. Food Chem. 48 (2000) 1160.
- Y. V. Pashin, L. M. Bakhitova, Environ. Health Perspect. 30 (1979) 185–189.
- US EPA, Compendium Method TO-13A, Cincinnati, OH (1999).
- European Commission Recommendation 2005/108/EC, Off. J. Eur. Comm. L34 (2005) 43.
- F. David, M. S. Klee, Agilent Publ. 5990-3451EN (2009).
- K. Lynam, D. Smith, Agilent Publ. 5989-9181EN (2008).
- R. Simon, S. Palme, E. Anklam, J. Chromatogr. A 1103 (2006) 307–313.
- L. R. Bordajandi et al., J. Sep. Sci. 31 (2008) 1769–1778.
- D. Rood, The Troubleshooting and Maintenance Guide for Gas Chromatographers, 4th Ed., Wiley-VCH (2007) p. 26.
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