Development of a three-dimensional porous ionic liquid-chitosan-graphene oxide aerogel for efficient extraction and detection of polyhalogenated carbazoles in sediment samples.

The three-dimensional porous ionic liquid-chitosan-graphene oxide aerogel (IL-CS-GOA) monolithic adsorbent with a through-hole structure was prepared using natural chitosan (CS) as the skeletal framework, graphene oxide (GO) as the support to provide mechanical strength, and ionic liquid (IL) as the porogen and modifier. The resulting IL-CS-GOA demonstrated a fluffy and porous structure with various pore sizes and excellent regeneration capability (over six cycles). Its specific surface area exceeded that of CS-GOA and IL-GOA by more than 7 times, enhancing its polyhalogenated carbazoles (PHCZs) adsorption capacity. Within 5 min, IL-CS-GOA (1.0 mg) exhibited adsorption amounts of 539 ng mg for 3-bromocarbazole (3-BCZ), 716 ng mg for 2,7-dibromocarbazole (2,7-BCZ), and 798 ng mg for 1,3,6,8-tetrabromocarbazole (1,3,6,8-BCZ), showcasing its rapid mass transfer and high adsorption capabilities. IL-CS-GOA was utilized as the adsorbent for glass dropper extraction (GDE) in conjunction with gas chromatography-mass spectrometry (GC-MS/MS), to develop a highly efficient and accurate method for determining PHCZs in sediments. Under optimal conditions, the established method exhibited a wide linear range (0.4-250 ng g, r ≥ 0.9990), low detection limits (0.04-0.24 ng g), and satisfactory recoveries (80.5 %-93.8 %), enabling the accurate and rapid detection of PHCZs in sediment samples. This study presents a novel approach for creating three-dimensional porous aerogels, introduces a new form of sample pretreatment using GDE with a monolithic adsorbent, and offers a new method for the determination of PHCZs in environmental matrices.