Organophosphorus pesticide and ester analysis by using comprehensive two-dimensional gas chromatography with flame photometric detection
2013
Liu, Xiangping | Li, Dengkun | Li, Jiequan | Rose, Gavin | Marriott, Philip J.
Thirty-seven phosphorus (P)-containing compounds comprising organophosphorus pesticides and organophosphate esters were analyzed by using comprehensive two-dimensional gas chromatography with flame photometric detection in P mode (GC×GC-FPD(P)), with a non-polar/moderately polar column set. A suitable modulation temperature and period was chosen based on experimental observation. A number of co-eluting peak pairs on the 1D column were well separated in 2D space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC×GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021–0.048μmolL−1, and linear calibration correlation coefficients (R2) for all 37 P-compounds were at least 0.998. The P-compounds were spiked in 2% diesel and good reproducibility for their response areas and retention times was obtained. Spiked recoveries were 88%–157% for 5μgL−1 and 80%–138% for 10μgL−1 spiked levels. Both 1tR and 2tR shifts were noted when the content of diesel was in excess of 5% in the matrix. Soil samples were analyzed by using the developed method; some P-compounds were positively detected. In general, this study shows that GC×GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples.
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