Rapid Chromatography for the Determination of Polychlorinated Biphenyls by GC-MS in Environmental Monitoring

Abstract

A method for determination of polychlorinated biphenyls (PCBs) in environmental and biological materials has been developed. This method includes rapid chromatography requiring less than 10 min using an HT-8 capillary column at 30 m × 0.25 mm i.d. Rapid chromatography was performed using a column temperature gradient from 80 to 310°C at a rate of 40°C/min. Low-resolution mass spectrometry in single ion monitoring mode of simultaneous detection of 12 target ions is suggested for detection of PCBs peaks. The method not only enabled us to reduce time of analysis but also to increase the efficiency of separating PCB peaks from interferences and to reduce levels of detection of analytes resulting in a minimized sample preparation stage. The last includes extraction of the PCBs using organic solvents, preliminary alkaline hydrolysis in the case of biological objects, and cleaning up the extracts on compact cartridges. The method was tested in monitoring studies for these contaminants in soils, sediments, snow cover, fish tissues, and seal blubber. Total PCBs and isomer congener groups of the same chlorination degree and seven indicator congeners (IUPAC No.'s 28, 52, 101, 118, 138, 153, and 180) are determined with a high degree of certainty. The PCB concentrations were in the range of 1–700 ng/g dry weight for environmental samples and 500–25000 ng/g lipids for biota. The method yields measurements of total PCBs and isomer groups with a precision no greater than 10% and no greater than 15% for the indicator congeners.

Keywords:

• Environmental monitoring
• Low-resolution mass spectrometry
• Polychlorinated biphenyls
• Rapid gas-chromatography

Acknowledgments

The authors express their appreciation to Dr. Elena V. Dzyuba, who provided us with biological samples.

Notes

Note. , where Δ₄₀ и Δ₃ are the errors of methods using high-rate and low-rate column heating (40 and 3°C/min respectively), d (%) is the discrepancy between results of the methods, and k = 21% is the control value for the discrepancy. LOD is the limit of detection.