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 x 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 D-1 column were well separated in D-2 space. Excellent FPD(P) detection selectivity, responding to compounds containing the P atom, produces clear 2D GC x GC plots with little interference from complex hydrocarbon matrices. Limits of detection (LOD) were within the range of 0.0021-0.048 mu molL(-1), and linear calibration correlation coefficients (R-2) 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 5 mu g L-1 and 80%-138% for 10 mu g L-1 spiked levels. Bothl (1)t(R) and (2)t(R) 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 x GC-FPD(P) is an accurate, sensitive and simple method for P-compound analysis in complicated environmental samples. (C) 2013 Elsevier B.V. All rights reserved.