Abstract
A method is described for multiple monolithic fiber solid-phase microextraction of five sterol and steroid hormones from complex food samples. A composite was prepared from graphene oxide, a metal-organic framework (ZIF-8) and a molecularly imprinted polymers was deposited on a single thin fiber. Four thin fibers were combined to obtain a fiber bundle. The nanocomposite was characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy. The parameters affecting the extraction were optimized by Box-Behnken design. Following elution with methanol, the analytes progesterone, testosterone, β-sitosterol, cholesterol and campesterol were quantified via HPLC. Response is linear in the 0.01–1000 μg L−1 concentration range, and limits of detection range from 3 to 5 ng L−1. The method was successfully applied to the determination of the five analytes in spiked samples of white meat, egg yolks and vegetables. The relative mean recoveries ranged from 95.0% to 101.0%.

Schematic presentation of a monolith molecularly imprinting polymer (MIP) fiber fabrication for solid phase microextraction (SPME) of sterol and steroid hormones. The fiber was synthesis using graphene oxide and metal-organic framework, ZIF-8, composite by imprinting technique and progesterone as template. Four fibers were combined to obtain a fiber bundle. Then, multiple fiber solid-phase microextraction was employed for determination of analytes by coupling with HPLC/UV detection.





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The Authors greatly appreciate the financial support of this work by Shahid Chamran University of Ahvaz Research Council.
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Mirzajani, R., Kardani, F. & Ramezani, Z. A nanocomposite consisting of graphene oxide, zeolite imidazolate framework 8, and a molecularly imprinted polymer for (multiple) fiber solid phase microextraction of sterol and steroid hormones prior to their quantitation by HPLC. Microchim Acta 186, 129 (2019). https://doi.org/10.1007/s00604-018-3217-4
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DOI: https://doi.org/10.1007/s00604-018-3217-4