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Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC × GC-TOFMS) is a technique highly suited for the separation and identification of complex mixtures such as petroleum.By the orthogonal column system, the structured separation was achieved.In the first non-polar dimension column, separation is mainly based on volatility of the analytes, whereas the separation in the second dimension polar column is mainly based on polarity.Time-of-flight mass spectrometry could provide structure information for the separated compounds.