Fully automated graphitic carbon nitride-based disposable pipette extraction-gas chromatography-mass spectrometric analysis of six polychlorinated biphenyls in environmental waters

A fully automated online emulsification-enhanced disposable pipette extraction-gas chromatography-mass spectrometry (EE-DPX-GC-MS) method has been developed for the extraction of six polychlorinated biphenyls (PCBs) from environmental waters. An in-house prepared material, graphitic carbon nitride (g-C3N4), was used as sorbent in a home-packed DPX device. The six PCBs studied include PCB 10, 28, 52, 153, 138 and 180. g-C3N4 was characterized successfully by X-ray diffraction, elemental analysis, scanning electron microscopy, Fourier-transform infrared and Raman spectroscopy. As a C-N analogue of graphite, the two-dimensional structure of g-C3N4 allows rapid analyte adsorption and desorption to take place. With a significant number of nitrogen functionalities in g-C3N4, the material dispersed well in aqueous sample, increasing the active surface area of contact between the sorbent and the sample. When coupled with a pre-emulsification step, PCBs in each portion of sample could be efficiently extracted by g-C3N4 within 20 s of gentle turbulence. Under the most favorable conditions, the automated online EE-DPX-GC-MS method achieved wide dynamic working ranges with good linearity (r(2) >= 0.998) for all analytes. Limits of detection ranging between 4.35 and 7.82 ng L-1 were attained, with enrichment factors of between 34 and 57 and relative standard deviations (RSDs) for intra- and inter-day precision of <= 8.95% and <= 12.6%, respectively. Absolute recoveries were between 69.3% and 109%. The fully automated online EE-DPX-GC-MS approach was applied to industrial wastewaters and reservoir waters where good relative recoveries of PCBs of between 89.3% and 105% were obtained, with RSDs <= 11.6%. (C) 2020 Elsevier B.V. All rights reserved.

Automated summary

A fully automated online method using emulsification-enhanced disposable pipette extraction-gas chromatography-mass spectrometry (EE-DPX-GC-MS) was developed for the extraction of six polychlorinated biphenyls (PCBs) from environmental waters. The use of graphitic carbon nitride as sorbent in a DPX device enabled rapid analyte adsorption and desorption, leading to high extraction efficiency. The method showed wide dynamic working ranges, good linearity, low detection limits, high enrichment factors, and good precision in both intra- and inter-day analysis.