Magnetic sorbents
based on iron–aluminum-mixed metal hydroxides
composited with metal–organic frameworks (MOFs) were designed
and synthesized using different benzoate ligands, including terephthalic
acid, 2-aminoterephthalic acid, 2,5-dihydroxyterephthalic acid, 1,3,5-benzenetricarboxylic
acid, and 1,2,4,5-benzenetetracarboxylic acid. The magnetic MOF derived
from terephthalic acid ligand exhibited an excellent extraction efficiency,
with adsorption capacities in the range of 2193–4196 mg kg
–1
, and was applied for magnetic solid-phase extraction
(MSPE) of carbamate pesticides, that is, bendiocarb, carbosulfan,
carbofuran, carbaryl, propoxur, isoprocarb, and promecarb. Simple
digital image colorimetry based on the diazotization reaction and
high-performance liquid chromatography (HPLC) were utilized for fast
screening and quantification purposes, respectively. A good analytical
performance for a simple screening approach using portable equipment
was obtained with detection limits in the range of 1.0–18.0
μg L
–1
. Under the optimized MSPE-HPLC conditions,
the entire developed procedure provided a wide linear range between
0.015 and 1000 μg L
–1
, low limits of detection,
and limits of quantitation ranging from 0.005 to 0.090 and 0.015–0.300
μg L
–1
, respectively. Enrichment factors up
to 184 were achieved. The intra- and interday relative standard deviations
were below 6.7 and 9.4%, respectively. The proposed MSPE-digital image
colorimetry and MSPE-HPLC methods were successfully applied for screening
and determining carbamate pesticides in fruits and vegetables. The
recoveries were obtained in a satisfactory range of 71.5–122.8%.
This discovery has led to the development of integration methods using
newly synthesized sorbent materials for the enrichment of carbamate
pesticides prior to their analysis in complicated samples. The developed
MSPE coupled with digital image colorimetry was efficient for fast
carbamate contamination screening, while MSPE-HPLC offered a sensitive
analytical methodology for quantifying contaminated samples.