This paper describes the development of a new design of hollow fiber solid/liquid phase microextraction (HF-SLPME) for determination of brilliant green (BG) residues in water fish ponds. This method consists of an aqueous donor phase and carbon nanotube reinforced organic solvent (acceptor phase) operated in direct immersion sampling mode. The multi-walled carbon nanotube dispersed in the organic solvent is held in the pores and lumen of a porous polypropylene hollow fiber. It is in contact directly with the aqueous donor phase. In this method the solid/liquid extractor phase is supported using a polypropylene hollow fiber membrane. Both ends of the hollow fiber segment are sealed with magnetic stoppers. This device is placed inside the donor solution and plays the rule of a pseudo-stir bar. It is disposable, so single use of the fiber reduces the risk of carry-over problems. Brilliant green (BG) after extraction from the aqueous samples with mentioned HF-SLPME device was determined by ultraviolet–visible spectroscopy with diode array detection (UV–vis/DAD). The absorption wavelength was set to 625nm (max). The effect of different variables on the extraction was evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The calibration curve was linear in the range of 1.00–10,000gL−1 of BG in the initial solution with R2 = 0.979. Detection limit, based on three times the standard deviation of the blank, was 0.55gL−1. All experiments were carried out at room temperature (25±0.5 ◦C).

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