Nitrobenzenes are widely used in industry for making dyes, pesticides, medicines, and explosives, and also used as intermediates in many chemistry syntheses. 1 There are several probable sources for nitrobenzenes in different matrices, including oil spills, industrial and municipal effluents, and atmospheric input. Nitrobenzenes are toxic; for example, the 14-day LC50 values toward the guppy (Poecilia reticulzata) are 12.5 mg l -1 for 2,4-DNT and 18 mg l -1 for 2,6-DNT. 2 Because of the ecotoxicology of nitrobenzenes and their ubiquitous existence in the environment, they become a risk or threat to both the growth of animals and the health of humans. For these reasons, nitrobenzenes have been included on the list of priority pollutants in water environment of China. 3 Therefore, it is imperative to develop rapid and simple methods for their determination in different matrices.For the aqueous samples, liquid-liquid extraction (LLE) is probably the most widely used sample preparation method. However, the main drawback of LLE is that it is timeconsuming and labor-intensive and requires a large amount of high-purity solvents, which are expensive and toxic. 4 SPE column needs pretreatment and still requires toxic organic solvents for the elution step, although solid-phase extraction (SPE) is less time-consuming than LLE.Solid-phase microextraction (SPME) is a solvent-free sample preparation method developed by Pawliszyn and his coworkers. 5 The technique is simple, rapid and easily operated, while it eliminates the disadvantages of conventional extraction methods, such as time-consuming operation and analytes loss. But SPME also suffers from some drawbacks: it is expensive and sample carry-over is also a problem.