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A novel mixed iron hydroxide molecularly imprinted polymer (MIH-MIP) was synthesized via polymerization using mixed-valence iron hydroxide as a magnetic supporter, glyphosate as a template, acrylamide as a functional monomer, and ethylene glycol dimethacrylate as a cross-linker. The resulting material was characterized and applied as a sorbent for the selective enrichment of glyphosate, aminomethylphosphonic acid, and glufosinate by magnetic solid-phase extraction (MSPE) prior to high-performance liquid chromatography. MIH-MIP possessed a high adsorption capacity in the range of 2.31–5.40 mg g–1 with good imprinting factors ranging from 1.52 to 7.59. The Langmuir model proved that the recognition sites were distributed as a monolayer on the surface of MIH-MIP. Scatchard analysis showed two types of binding sites on MIH-MIP. The kinetic characteristics of MIH-MIP suggested that the binding process of all analytes fit well with the pseudosecond-order model. The developed methodology provides good linearity in the range of 72.0–2000.0 μg L–1. Low detection limits of 21.0–22.5 μg L–1 and enrichment factors of up to 18 were achieved. The precision in terms of relative standard deviations of the intra- and interday experiments was better than 7 and 9%, respectively. The applicability of the developed MSPE facilitates the accurate and efficient determination of water, soil, and vegetable samples with satisfactory recoveries in the range of 86–118%. The results confirmed the suitability of the MIH-MIP sorbent for selective extraction and quantification of glyphosate, aminomethylphosphonic acid, and glufosinate.

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