Nanosheets of a porous layered double hydroxide were directionally arranged on boehmite nanowires and porous carbon and used as a coating for solid-phase microextraction (SPME) method. Porous carbon tubes were prepared from goat grass and then coated with layered double hydroxide nanosheets and boehmite nanowires. The nanomaterial was placed on a stainless-steel wire which then was used for the extraction of fifteen agrochemicals from aqueous sample solutions. The extraction temperature, extraction time, ionic strength, stirring rate, and desorption temperature and time were optimized. Following thermal desorption of the agrochemicals in the injector of the gas chromatograph, they were quantified by GC/MS. Under optimum conditions, the repeatability for one fiber, expressed as relative standard deviation, was between 2.9 and 11.1%. The detection limits for the agrochemicals are between 2–29 ng L−1. The method is simple, fast, and inexpensive (in terms of equipment). The fiber is thermally stable, and the relative recoveries from spiked samples are better compared to conventional methods of extraction
