The synthesis of a nanocomposite
based on molecularly imprinted poly(methacrylic acid) (MIP) grafted
on an iniferter-modified carbon nanotube (MIP/MWCNT) by living-radical
polymerization and its application for 17β-estradiol (E2) adsorption
is described. The nonimprinted nanocomposite (NIP/MWCNT) and the polymers
MIP and NIP synthesized in the absence of carbon nanotubes were also
prepared and characterized by FT-IR, TGA, nitrogen adsorption–desorption
measurements, and SEM and TEM techniques. From TEM images, a narrow
layer of MIP at nanoscale onto MWCNT surface was formed, as expected
by iniferter-controlled synthesis. The adsorption capacity of MIP/MWCNT
toward E2 was higher than MIP. In addition, relative selectivity coefficients
(k′) higher than one unit were obtained from
competitive adsorption studies in the presence of estrone, 17α-ethynylestradiol,
and bisphenol A, thereby demonstrating that MIP/MWCNT is more selective
toward E2 when compared to NIP/MWCNT. Equilibrium adsorption of E2
was reached at 120 min and the maximum adsorption capacity of the
nanocomposite was found to be 40.0 mg g–1, showing
higher or similar performance when compared with others adsorbent
materials described on the literature for E2. Thermodynamic parameters
suggest that the adsorption process is spontaneous and of exothermic
nature. The performance of MIP/MWCNT as a new packing adsorbent material
was evaluated for E2 extraction in solid-phase extraction (SPE) procedure,
which was performed by loading the sample at pH 7.0 through 50.0 mg
of MIP/MWCNT packed into SPE cartridge. Taking into account the high
elution value of 96 ± 3.6% obtained by using acetone:chloroform
(1:1 v/v), as well as the selectivity of adsorbent, we can infer that
MIP/MWCN/T nanocomposite shows interesting analytical potentiality
for E2 preconcentration from natural water samples.
This paper describes the development of a new electrochemical sensor for 17β‐estradiol (E2) determination based on glassy carbon electrode (GCE) modified with molecularly imprinted polymer grafted onto iniferter‐multiwall carbon nanotubes surface (MIP‐MWCNT) and dihexadecyl‐hydrogen‐phosphate (DHP). The electrochemical method was based on closed‐circuit preconcentration of E2 in 0.1 mol L−1 phosphate buffer (pH 7.0) during 500 s. Upon preconcentration, E2 was determined by differential pulse voltammetry (DPV) exhibiting a limit of detection of 0.01 μmol L−1. The sensor exhibited higher selectivity toward E2 and it was applied for E2 determination in natural water samples, with accuracy attested by HPLC‐DAD.
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