Micro-matrix cartridge extraction followed by online micro-solid phase extraction based on polystyrene@hydroxypropyl-β-cyclodextrin nanofibers for selective determination of fipronil and its metabolites in soil

作者：Liu, Ying; Hou, Shenghuai; Chen, Tiantian; Li, Yan; Zhang, Manlin; Zhou, Dandan; Xu, Hui^*

来源：Mikrochimica Acta, 2023, 190(4): 138.

DOI：10.1007/s00604-023-05714-1

• Fipronil
• Fipronil metabolites
• Soil analysis
• Micro-matrix cartridge extraction
• Online-micro-solid phase extraction
• HPLC-MS
• PS@HPCD nanofibers

Micro-matrix cartridge extraction coupled on-line to micro-solid phase extraction-high performance liquid chromatography-mass spectrometry (mu-MCE-online-mu-SPE-HPLC-MS) is presented. Micro-matrix cartridge extraction (mu-MCE) was applied to highly efficient desorption of adsorbed pesticides from contaminated soil with favorable extraction efficiency (100%). Novel polystyrene@hydroxypropyl-beta-cyclodextr in (PS@HPCD) electrospun nanofibers with 3D network structure were prepared to selectively capture fipronil and its metabolites. High selectivity was obtained with adsorption efficiency >= 86.64% via complexation, hydrophobic affinity, and pi-pi interactions. PS@HPCD nanofibers exhibited remarkable advantages such as excellent enrichment factors (24-55), superior permeability, and long service life (> 65 times). Under the optimum conditions, wide linear range (0.1-1000 ng g(-1)), low detection limits (0.0032-0.0067 ng g(-1)), high recoveries (84-124.5%), favorable repeatability (RSD <= 10.4%, n = 5), and reproducibility (RSD < 7.2%, n = 3) were acquired for fipronil and three metabolites. The developed method was applied to the pesticide determination in actual soils and the ISO-certified soil with satisfactory recoveries (96.5%). The method developed provides a green, efficient, and miniaturized method for the determination of trace pesticide residues in soil.