Preparation of Acryloyl β -Cyclodextrin Organic Polymer Monolithic Column and Its Application in Solid-Phase Microextraction and HPLC Analysis for Carbofuran and Carbaryl in Rice

An acryloyl β -cyclodextrin (A- β -CD) monolithic column for solid-phase microextraction (SPME) and determination of carbofuran and carbaryl by high-performance liquid chromatography (HPLC) have been prepared through a “one-step” polymerization method. The synthesis conditions, including the volume of cross-linker, the ratio and volume of mixed porogenic solvent consisted of methanol and N,N -dimethylformamide were optimized. The prepared monolithic column was characterized by thermogravimeteric analysis (TGA), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and Brunner-Emmet-Teller (BET) measurement. The eluent type, volume and flow rate, sample volume, flow rate, acidity, and ionic strength were optimized in detail. Under the optimized conditions, a simple, rapid, and sensitive SPME-HPLC method was developed for determination of carbofuran and carbaryl in rice samples. The method yielded a linear calibration curve in the concentration ranges of 1.5–200 μg/kg for carbofuran and 0.3–200 μg/kg for carbaryl with correlation coefficients ( R 2 ) of above 0.9955. Limits of detection ( S / N = 3) were 0.5 μg/kg for carbofuran and 0.1 μg/kg for carbaryl, respectively. The recoveries of this method ranged from 88.1 to 105.8%. The relative standard deviations were less than 8.1%.