Development of MIL-101(Fe)/Silica Aerogel Nanohybrid for Chlorpyrifos Extraction in Soil Using Magnetic Fiber Headspace Solid-Phase Microextraction Combined with Gas Chromatography-Mass Spectrometry

Abstract

A hybrid material combining silica aerogel with MIL-101(Fe) was synthesized and effectively utilized as a fiber coating for the headspace solid-phase microextraction of Chlorpyrifos. The nanohybrid was characterized using a range of analytical techniques. Employing a magnetic field, generated with a pair of permanent disc magnets, on the coated steel fiber significantly enhanced the extraction efficiency for the majority of the target components. Optimization of key parameters influencing the extraction performance was conducted using a one-variable-at-a-time approach. The optimized conditions included a temperature of 120 °C, water addition of 10 µL, and an extraction time of 10 minutes. The prepared fiber demonstrated stability and could be reused multiple times without noticeable deterioration in efficiency. For precision assessment, five repeat analyses were carried out, yielding a relative standard deviation (RSD) of 5.1% for peak areas associated with the target compound. Furthermore, the method proved highly reliable and effective when applied to real-world scenarios, successfully extracting and identifying Chlorpyrifos from soil samples. The results highlight the robustness, reproducibility, and practical utility of this innovative approach in analytical applications.