Abstract

Poly(phenyl-(4-(6-thiophen-3-yl-hexyloxy)-benzylidene)-amine) (P3TArH) was successfully synthesized and coated on the surface of Fe3O4 magnetic nanoparticles (MNPs). The nanocomposites were characterized by Fourier transform infra-red (FTIR), X-ray diffractometry (XRD), Brunauer-Emmett-Teller (BET) surface area analysis, analyzer transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM). P3TArH-coated MNPs (MNP@P3TArH) showed higher capabilities for the extraction of commonly-used phthalates and were optimized for the magnetic-solid phase extraction (MSPE) of environmental samples. Separation and determination of the extracted phthalates, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), dipropyl phthalate (DPP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dicyclohexyl phthalate (DCP), di-ethylhexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP), were conducted by a gas chromatography-flame ionization detector (GC-FID). The best working conditions were as follows; sample at pH 7, 30 min extraction time, ethyl acetate as the elution solvent, 500-µL elution solvent volumes, 10 min desorption time, 10-mg adsorbent dosage, 20-mL sample loading volume and 15 g·L−1 concentration of NaCl. Under the optimized conditions, the analytical performances were determined with a linear range of 0.1–50 µg·L−1 and a limit of detection at 0.08–0.468 µg·L−1 for all of the analytes studied. The intra-day (n = 7) and inter-day (n = 3) relative standard deviations (RSD%) of three replicates were each demonstrated in the range of 3.7–4.9 and 3.0–5.0, respectively. The steadiness and reusability studies suggested that the MNP@P3TArH could be used up to five cycles. The proposed method was executed for the analysis of real water samples, namely commercial bottled mineral water and bottled fresh milk, whereby recoveries in the range of 68%–101% and RSD% lower than 7.7 were attained.

Highlights

  • Belonging to non-halogenated esters of phthalic acid, phthalates or phthalate esters are used as plasticizers for nitrocellulose, since it was first recognized in 1880, replacing camphor [1]

  • Exposure to phthalates over long-term periods could result in health issues, for example potential carcinogenic effects or critical impact on the hormonal systems, since they own lipophilic properties, which make them stored in fatty tissues [7,8,9,10]

  • The optimized method obtained for the extraction of phthalates using magnetic nanoparticles (MNPs)@P3TARH involved the sample at pH 7, 30 min extraction time, ethyl acetate as the elution solvent, 500-μL elution solvent volumes, 10 min desorption time, 10 mg adsorbent dosage, 20-mL sample loading volume and a 15 g L1 concentration of NaCl

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Summary

Introduction

Belonging to non-halogenated esters of phthalic acid, phthalates or phthalate esters are used as plasticizers for nitrocellulose, since it was first recognized in 1880, replacing camphor [1]. Other consumer-based products utilizing phthalates are as a component in inks, adhesive materials, lacquers, sealing and packing materials, materials for treating surfaces, solvents and fixing agents in fragrances, as well as additives in cosmetics [3,4,5]. They become emerging pollutants and harmful to humans, especially children, since they are not chemically bound in plastics. The usage of phthalates in the production of toys, baby bottles and pacifiers is banned in many countries [6]. In Malaysia, due to the awareness of the migration of phthalates from food packaging, baby bottles and pacifiers, a regulation has been proposed, which in stated in Food Regulation

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