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. 2019 Nov 16;5(11):e02848.
doi: 10.1016/j.heliyon.2019.e02848. eCollection 2019 Nov.

Evaluation of metal-organic framework NH2-MIL-101(Fe) as an efficient sorbent for dispersive micro-solid phase extraction of phenolic pollutants in environmental water samples

Tittaya Boontongto  1 , Rodjana Burakham  1
Affiliations

Evaluation of metal-organic framework NH2-MIL-101(Fe) as an efficient sorbent for dispersive micro-solid phase extraction of phenolic pollutants in environmental water samples

Tittaya Boontongto et al. Heliyon. .

Abstract

This work proposes an application of amine-functionalized metal-organic framework (NH2-MIL-101(Fe)) as sorbent for dispersive micro-solid phase extraction (D-μSPE) of ten priority phenolic pollutants. The sorbent was simply synthesized under facile condition. The entire D-μSPE process was optimized by studying the effect of experimental parameters affecting the extraction recovery of the target analytes. The final extract was analyzed using high performance liquid chromatography with photodiode array detector. Under the optimum condition, the proposed procedure can be applied for wide linear calibration ranges between 1.25-5000 μg L-1 with the correlation coefficients of greater than 0.9900. The limits of detection (LODs) and limits of quantitation (LOQs) were in the ranges of 0.4-9.5 μg L-1 and 1.25-30 μg L-1, respectively. The precision evaluated in terms of the relative standard deviations (RSDs) of the intra- and inter-day determinations of the phenol compounds at their LOQ concentrations were below 13.9% and 12.2%, respectively. High enrichment factors up to 120 were reached. The developed method has been successfully applied to determine phenol residues in environmental water samples. The satisfactory recoveries obtained by spiking phenol standards at two different concentrations (near LOQs and 5 times as high as LOQs) ranged from 68.4-114.4%. The results demonstrate that the NH2-MIL-101(Fe) material is promising sorbent in the D-μSPE of phenolic pollutants.

Keywords: Analytical chemistry; Dispersive solid-phase extraction; Environmental science; HPLC; Metal-organic framework; Phenol.

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Figures

Fig. 1
Fig. 1
Schematic diagram of the proposed D-μSPE procedure for determination of phenolic pollutants.
Fig. 2
Fig. 2
XRD patterns of the synthesized NH2-MIL-101(Fe) and simulated MIL-101.
Fig. 3
Fig. 3
FTIR spectra of the synthesized NH2-MIL-101(Fe).
Fig. 4
Fig. 4
SEM images of as-synthesized NH2-MIL-101(Fe).
Fig. 5
Fig. 5
Effect of sorbent amount on D-μSPE of phenolic pollutants.
Fig. 6
Fig. 6
Effect of eluent type on D-μSPE of phenolic pollutants.
Fig. 7
Fig. 7
Effect of eluent volume on D-μSPE of phenolic pollutants.
Fig. 8
Fig. 8
Effect of vortex adsorption time on D-μSPE of phenolic pollutants.
Fig. 9
Fig. 9
Effect of centrifugation time after adsorption on D-μSPE of phenolic pollutants.
Fig. 10
Fig. 10
Effect of vortex desorption time on D-μSPE of phenolic pollutants.
Fig. 11
Fig. 11
Effect of centrifugation time after desorption on D-μSPE of phenolic pollutants.
Fig. 12
Fig. 12
Chromatograms obtained from direct HPLC and D-μSPE-HPLC process. Peak assignment: 1, Ph; 2, 4NP; 3, 2CP; 4, 24DNP; 5, 2NP; 6, 24DMP; 7, 4C3MP; 8, 24DCP; 9, 2M46DNP; 10, 246TCP (concentration: 500 μg L−1 for D-μSPE-HPLC and 7000 μg L−1 for direct HPLC).
Fig. 13
Fig. 13
XRD patterns of simulated MIL-101(Fe), MIL-101 (Fe) before and after adsorption of phenol standards in aqueous solution.
Fig. 14
Fig. 14
Comparison of adsorption ability between NH2-MIL-101(Fe) and MIL-101(Fe) using 2 mg L−1 of each phenol standards.
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