Application of β-Cyclodextrin metal-organic framework/titanium dioxide hybrid nanocomposite as dispersive solid-phase extraction adsorbent to organochlorine pesticide residues in honey samples

Abstract

A simple and efficient dispersive solid-phase extraction (D-SPE) method combined with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed to determine organochlorine pesticides (OCP) in honey. Firstly, a type of hybrid nanocomposite (CD-MOF/TiO₂) was prepared by grafting a metal-organic framework material synthesized with cyclodextrin as an organic ligand onto titanium dioxide. Then, the CD-MOF/TiO₂ was used as a D-SPE adsorbent to extract the OCP, and the effects of the amount of adsorbent, ultrasonic time, vortex time, pH, and salinity on the extraction were investigated using Plackett–Burman design and Box-Behnken Design. Under the optimized adsorption and desorption conditions, an analysis method that combined D-SPE with GC-MS/MS was established. The linear ranges of 14 OCP are 1–500 μg kg⁻¹ and the correlation coefficients are between 0.9991 and 1.000. The limits of detection and quantification vary from 0.01 to 0.04 μg kg⁻¹ and 0.04 to 0.12 μg kg⁻¹, respectively. The intra-day and inter-day precision of this method are suitable (RSDs% less than 11.3%). The established CD-MOF/TiO₂ / D-SPE method was used for the extraction of OCP in honey samples with recovery in the range of 76.4 to 114.3%. The results demonstrate that the CD-MOF/TiO₂ has a good selective enrichment ability for OCP and is suitable for the D-SPE pretreat of honey sample analysis.