ABSTRACT
Herein, a novel polypyrrole-polyaniline functionalized magnetic porous carbon (MPC@PPy-PANI) composite material was fabricated and utilized for the separation/extraction of furfurals from baby food and dry milk samples. In this way, magnetite@silica nanoparticles were first synthesized, and then a magnetic metal-organic framework (MMIL-101(Fe)) was prepared. After that, the MMIL-101(Fe) was pyrolyzed in a neutral atmosphere to obtain MPC. Ultimately, the MPC was functionalized with a co-polymer of aniline-pyrrole via oxidation polymerization. The synthesis of MPC@PPy-PANI was confirmed with FT-IR spectroscopy, SEM, TEM, VSM, and XRD techniques. Furfural and hydroxymethyl furfural were selected as the model analytes, which were separated/quantified on an HPLC-UV instrument. The LODs, LOQs, and linear dynamic ranges (LDRs) were in the range of 0.3-0.7 µg kg-1, 1.0-2.5 µg kg-1, and 1.0-600 µg kg-1, respectively. Repeatability of the method was studied as an RSD parameter, and was located in the range of 5.5-6.8% (within-day, n = 5) and 8.2-9.4% (between-day, n = 3 days). The applicability of the proposed method was established by analyzing several baby food and dry milk samples. The relative recovery (RR%) and repeatability were located in the range of 86-111% and 3.3-10.1%, respectively, showing excellent accuracy and precision of the method.
ABSTRACT
The aim of the current research is to develop a MSPE method for the determination of furfural in baby food and dry milk samples. In this regard, a novel magnetic porous carbon composite coated with poly(p-phenylenediamine) was fabricated, characterized, and then applied to the preconcentration/extraction of furfurals from baby food and dry milk powder samples. Initially, magnetic nanoparticles (Fe3O4) were synthesized, and then coated with a metal-organic framework layer named MIL-101(Fe). Afterward, the magnetic MIL-101(Fe) was subjected to calcination under a nitrogen atmosphere and magnetic porous carbon was achieved. Finally, a layer of poly(p-phenylenediamine) was coated on the magnetic porous carbon. The structure of the nanocomposite was investigated with various methods, including FT-IR spectroscopy, electron microcopies (SEM and TEM), VSM, and XRD. The fabricated nanocomposite was applied in magnetic solid-phase extraction of furfural and hydroxymethyl furfural and their determination with liquid chromatography. The effect of experimental variables was explored by using an experimental design approach. The LODs and linear range for the target furfurals were 1.0-2.0 µg kg-1 and 3.0-500 µg kg-1, respectively. The method's repeatability was explored using RSD values and was found to be in the range of 5.2-6.4% (one-day, n = 5) and 9.1-10.8% (day to day, n = 3). Eventually, this new method was employed for the extraction/quantification of target compounds in baby food and dry milk powder samples.
