PAH Analyses with High Efficiency GC Columns: Column Selection and Best Practices
Applications | 2010 | Agilent TechnologiesInstrumentation
Polycyclic aromatic hydrocarbons (PAHs) are widespread environmental and food contaminants formed during incomplete combustion of organic matter. Many PAHs are classified as mutagenic or carcinogenic, and regulatory bodies in the European Union (EU) and the U.S. Environmental Protection Agency (EPA) maintain priority lists for monitoring food, environmental samples, and consumer exposure. Rapid, reliable analysis of these regulated PAHs is essential for food safety, environmental monitoring, and public health.
This study aimed to optimize gas chromatography–mass spectrometry (GC–MS) methods to separate and quantify all 24 PAHs combined from the EU 15+1 list and the EPA list within minimal analysis time. Two high-efficiency capillary columns from Agilent Technologies—DB-EUPAH (20 m × 0.18 mm, 0.14 µm) and DB-5ms (20 m × 0.18 mm, 0.18 µm)—were evaluated for their ability to resolve critical isomer pairs and accelerate throughput.
Standards for the EU and EPA PAH mixtures were each prepared at 2 µg/mL, mixed 1:1, and injected (0.5 µL) in splitless mode. Helium carrier gas (constant flow, 1.8 mL/min) and temperature programs tailored to each column supported rapid elution of low- to high-boiling PAHs. Mass detection employed an Agilent 5975C MSD in SIM/Scan mode (50–400 amu) with source and transfer line temperatures at 340 °C.
The DB-EUPAH column achieved baseline resolution of all 24 regulated PAHs—including the challenging benzo[b,j,k]fluoranthene isomers—in under 28 minutes. Its midpolar phase and high-temperature tolerance also improved peak shapes for high-molecular-weight dibenzopyrene isomers. The DB-5ms column resolved 23 of the 24 PAHs (benzo[j]fluoranthene and benzo[k]fluoranthene coelute) but completed analysis in under 22 minutes, offering a 27 % faster cycle when isomer separation is not required.
Advances in GC column materials and designs will continue to improve PAH separations, especially for high-mass isomers. Integration of retention gaps, inlet backflushing, and elevated linear velocities can further accelerate analyses. Emerging mass spectrometry detectors and data processing algorithms may enhance selectivity and quantitation of trace-level PAHs in complex matrices.
High-efficiency Agilent DB-EUPAH and DB-5ms columns enable robust GC–MS analysis of EU 15+1 and EPA PAH priorities. DB-EUPAH delivers full isomer resolution in <28 minutes, while DB-5ms offers faster throughput (≤22 minutes) for summed isomer reporting. These optimized methods support regulatory compliance and high-throughput environmental or food safety testing.
1. Mottier P., Parisod V., Turesky R.J. J. Agric. Food Chem. 48 (2000):1160.
2. Pashin Y.V., Bakhitova L.M. Environ. Health Perspect. 30 (1979):185–189.
3. European Commission Recommendation 2005/108/EC. Off. J. Eur. Comm. L34 (2005):43.
4. U.S. EPA Compendium Method TO-13A, EPA, Cincinnati, OH, USA, 1999.
5. David F., Klee M.S. Agilent Publ. 5990-3451EN (2009).
6. Lynam K., Smith D. Agilent Publ. 5989-9181EN (2008).
7. Gomez-Ruiz J.A., Wenzl T. Anal. Bioanal. Chem. 393 (2009):1697–1707.
8. Bordajandi L.R., Dabrio M., Ulberth F., Emons H. J. Sep. Sci. 31 (2008):1769–1778.
9. Smith D., Lynam K. Agilent Publ. 5990-4883EN (2009).
GC/MSD, GC/SQ, GC columns, Consumables
IndustriesEnvironmental, Food & Agriculture
ManufacturerAgilent Technologies
Summary
Significance of the Topic
Polycyclic aromatic hydrocarbons (PAHs) are widespread environmental and food contaminants formed during incomplete combustion of organic matter. Many PAHs are classified as mutagenic or carcinogenic, and regulatory bodies in the European Union (EU) and the U.S. Environmental Protection Agency (EPA) maintain priority lists for monitoring food, environmental samples, and consumer exposure. Rapid, reliable analysis of these regulated PAHs is essential for food safety, environmental monitoring, and public health.
Objectives and Study Overview
This study aimed to optimize gas chromatography–mass spectrometry (GC–MS) methods to separate and quantify all 24 PAHs combined from the EU 15+1 list and the EPA list within minimal analysis time. Two high-efficiency capillary columns from Agilent Technologies—DB-EUPAH (20 m × 0.18 mm, 0.14 µm) and DB-5ms (20 m × 0.18 mm, 0.18 µm)—were evaluated for their ability to resolve critical isomer pairs and accelerate throughput.
Instrumental Methodology and Chromatographic Conditions
Standards for the EU and EPA PAH mixtures were each prepared at 2 µg/mL, mixed 1:1, and injected (0.5 µL) in splitless mode. Helium carrier gas (constant flow, 1.8 mL/min) and temperature programs tailored to each column supported rapid elution of low- to high-boiling PAHs. Mass detection employed an Agilent 5975C MSD in SIM/Scan mode (50–400 amu) with source and transfer line temperatures at 340 °C.
Used Instrumentation
- GC: Agilent 7890A with backflush capability
- MSD: Agilent 5975C Series
- Autosampler: Agilent 7873B liquid sampler
- Columns: DB-EUPAH (20 m×0.18 mm, 0.14 µm) and DB-5ms (20 m×0.18 mm, 0.18 µm)
- Consumables: amber vials, septa, deactivated inlet liners, vespel/graphite ferrules
Main Results and Discussion
The DB-EUPAH column achieved baseline resolution of all 24 regulated PAHs—including the challenging benzo[b,j,k]fluoranthene isomers—in under 28 minutes. Its midpolar phase and high-temperature tolerance also improved peak shapes for high-molecular-weight dibenzopyrene isomers. The DB-5ms column resolved 23 of the 24 PAHs (benzo[j]fluoranthene and benzo[k]fluoranthene coelute) but completed analysis in under 22 minutes, offering a 27 % faster cycle when isomer separation is not required.
Benefits and Practical Applications
- Comprehensive coverage of EU and EPA regulated PAHs for food and environmental labs
- Flexible column choice based on resolution needs versus speed
- High-efficiency narrow-bore columns reduce run times without sacrificing sensitivity
- Optimized injection and system parameters lower detection limits and maintenance frequency
Future Trends and Applications
Advances in GC column materials and designs will continue to improve PAH separations, especially for high-mass isomers. Integration of retention gaps, inlet backflushing, and elevated linear velocities can further accelerate analyses. Emerging mass spectrometry detectors and data processing algorithms may enhance selectivity and quantitation of trace-level PAHs in complex matrices.
Conclusion
High-efficiency Agilent DB-EUPAH and DB-5ms columns enable robust GC–MS analysis of EU 15+1 and EPA PAH priorities. DB-EUPAH delivers full isomer resolution in <28 minutes, while DB-5ms offers faster throughput (≤22 minutes) for summed isomer reporting. These optimized methods support regulatory compliance and high-throughput environmental or food safety testing.
References
1. Mottier P., Parisod V., Turesky R.J. J. Agric. Food Chem. 48 (2000):1160.
2. Pashin Y.V., Bakhitova L.M. Environ. Health Perspect. 30 (1979):185–189.
3. European Commission Recommendation 2005/108/EC. Off. J. Eur. Comm. L34 (2005):43.
4. U.S. EPA Compendium Method TO-13A, EPA, Cincinnati, OH, USA, 1999.
5. David F., Klee M.S. Agilent Publ. 5990-3451EN (2009).
6. Lynam K., Smith D. Agilent Publ. 5989-9181EN (2008).
7. Gomez-Ruiz J.A., Wenzl T. Anal. Bioanal. Chem. 393 (2009):1697–1707.
8. Bordajandi L.R., Dabrio M., Ulberth F., Emons H. J. Sep. Sci. 31 (2008):1769–1778.
9. Smith D., Lynam K. Agilent Publ. 5990-4883EN (2009).
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