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. 2022 Oct 10;12(44):28728-28737.
doi: 10.1039/d2ra02916b. eCollection 2022 Oct 4.

UiO-66-based metal-organic framework for dispersive solid-phase extraction of vanillylmandelic acid from urine before analysis by capillary electrophoresis

Roghayeh Hassanpour-Sabet  1 , Behruoz Seyfinejad  2   3 , Elnaz Marzi Khosrowshahi  1 , Mahboob Nemati  1 , Mohammad Reza Afshar Mogaddam  1   2 , Abolghasem Jouyban  2   4
Affiliations

UiO-66-based metal-organic framework for dispersive solid-phase extraction of vanillylmandelic acid from urine before analysis by capillary electrophoresis

Roghayeh Hassanpour-Sabet et al. RSC Adv. .

Abstract

Dispersive solid-phase extraction (DSPE) was developed for the extraction of vanillylmandelic acid (VMA) in urine samples prior to capillary electrophoresis with diode array detection (CE-DAD). Extraction of VMA by DSPE was carried out by direct addition of 7.5 mg of synthesized amino-functionalized UiO-66 (Zr) metal-organic framework adsorbent into the 5 mL sample solution (pH 4.0), followed by sonication and centrifugation. The supernatant layer was discarded, then the sedimented adsorbent was eluted using borate buffer (75 mM, pH 10). Effective extraction parameters including the amount of adsorbent, sample pH, adsorption and desorption time, type, volume and pH of eluent, and type of adsorbent dispersion method were systematically investigated. Under the optimized conditions, linearity of the method was from 40 to 2000 μg L-1 with a correlation coefficient over 0.9948. The method detection and quantification limits were 12 and 40 μg L-1, respectively. The relative standard deviations for intra-and inter-day precision were 2.4 and 2.8% (n = 5), respectively. The extraction recovery and enrichment factor values were 90% and 9.0 respectively.

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Conflict of interest statement

The authors declare that they have no conflict of interest.

Figures

Fig. 1
Fig. 1. (a) Nitrogen adsorption/desorption isotherm (b) UV-vis spectrum, (c) XRD pattern, and (d) FTIR spectrum of the MOF.
Fig. 2
Fig. 2. The effect of affective variables in the adsorption step on DSPE of VMA; effects of sample pH, (A) adsorbent amount, (B) sample agitation type, (C) adsorption time, (D) and salt addition. (E) The error bars indicate minimum and maximum values of three independent determinations.
Fig. 3
Fig. 3. The effect of affective variables in the desorption step on DSPE of VMA; effects of sample agitation type, (A) adsorption time, (B) eluent type, (C) eluent volume, (D) and eluent concentration. (E) The error bars indicate minimum and maximum values of three independent determinations.
Fig. 4
Fig. 4. Typical electropherogram of urine #1 sample (a) before and (b) after spike with 100 μg L−1 of VMA.
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