Abstract
Herein, cellulose acetate membrane modified with polyethylene terephthalate derived MIL-101(Fe)
(PET-MIL-101(Fe)) was used as an extraction phase for the direct immersion-thin film microextraction
method (DI-TFME) of neonicotinoid insecticides in water samples. The quantitative analysis of
clothianidin, imidacloprid, thiacloprid and thiamethoxam was carried out using high-pressure liquid
chromatography (HPLC-DAD). The morphological and structural characteristics of the materials were
studied using transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), and energy
dispersive X-ray spectrometry (EDX). Under optimum conditions, acceptable analytical performance
for the developed DI-TFME/HPLC-DAD method was attained. The linearity of the method ranged from
0.04 to 500 μg/L with R2 ranging from 0.9981 to 0.9989. The detection limits, quantification limits and
relative standard deviation (%RSD) of the DI-TFME/HPLC-DAD method were in the range of 0.013–
0.016 μg/L, 0.043–0.053 μg/L and 1.2–3.9%, respectively. The method was applied in the analysis of
real water samples, and the spiking recoveries of the target analytes were 95.6–102%, 91.2–98.6%
and 79.2‒98.7% for river water, effluent and influent samples, respectively, with %RSDs ranging from
1.8 to 4.8%. These findings demonstrated that the developed DI-TFME/HPLC-DAD method had high
precision, accuracy, sensitivity and enrichment factor (73–88). The DI-TFME/HPLC-DAD method proved
sustainable for the simultaneous quantification of trace neonicotinoid insecticides in real samples.