In this work, the synthesis, characterization, and application of novel parabens imprinted polymers as highly selective solid-phase extraction (SPE) sorbents have been reported. The imprinted polymers were created using sol–gel molecular imprinting process. All the seven parabens were considered herein in order to check the phase selectivity. By means of a validated HPLC-photodiode array detector (PDA) method all seven parabens were resolved in a single chromatographic run of 25 min. These SPE sorbents, in-house packed in SPE empty cartridges, were first characterized in terms of extraction capability, breakthrough volume, retention volume, hold-up volume, number of theoretical plates, and retention factor. Finally, the device was applied to a real urine sample to check the method feasibility on a very complex matrix. The new paraben imprinted SPE sorbents, not yet present in the literature, potentially encourage the development of novel molecularly imprinted polymers (MIPs) to enhance the extraction efficiency, and consequently the overall analytical performances, when the trace quantification is required.
This paper reports the performance comparison between the exhaustive and equilibrium extraction using classical Avantor C18 solid phase extraction (SPE) sorbent, hydrophilic-lipophilic balance (HLB) SPE sorbent, Sep-Pak C18 SPE sorbent, novel sol-gel Carbowax 20M (sol-gel CW 20M) SPE sorbent, and sol-gel CW 20M coated fabric phase sorptive extraction (FPSE) media for the simultaneous extraction and analysis of three inflammatory bowel disease (IBD) drugs that possess logP values (polarity) ranging from 1.66 for cortisone, 2.30 for ciprofloxacin, and 2.92 for sulfasalazine. Both the commercial SPE phases and in-house synthesized sol-gel CW 20M SPE phases were loaded in SPE cartridges and the extractions were carried out under an exhaustive extraction mode. FPSE was carried out under an equilibrium extraction mode. The drug compounds were resolved using a Luna C18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode within 20 min and the method was validated in compliance with international guidelines for the bioanalytical method validation. Novel in-house synthesized and loaded sol-gel CW 20M SPE sorbent cartridges were characterized in terms of their extraction capability, breakthrough volume, retention volume, hold-up volume, number of the theoretical plate, and the retention factor.
Poly(methyl methacrylate) (PMMA) is characterized by high CO2 capture yield under mild pressures and temperatures. A morphological modification of powdery amorphous PMMA (pPMMA) is carried out by electrospinning to increase the surface/volume ratio of the resulting electrospun PMMAs (ePMMAs). This modification improves the kinetics and the capture yields. The rate constants observed for ePMMAs are two to three times higher than those for pPMMA, reaching 90% saturation values within 5–7 s. The amount of sorbed CO2 is up to eleven times higher for ePMMAs at 1 °C, and the highest difference in captured CO2 amount is observed at the lowest tested pressure of 1 MPa. The operating life of the ePMMAs shows a 5% yield loss after ten consecutive runs, indicating good durability. Spent electrospun PMMAs after several cycles of CO2 sorption-desorption can be regenerated by melting and again electrospinning the molten mass, resulting in a CO2 capture performance that is undistinguishable from that observed with fresh ePMMA. Scanning electron and atomic force microscopies show a reduction in surface roughness after gas exposure, possibly due to the plasticization effect of CO2. This study shows the potential of electrospun PMMAs as solid sorbents for carbon capture from natural gas or pre-combustion and oxyfuel combustion processes.