Determination of phthalate esters in drinking water and edible vegetable oil samples by headspace solid phase microextraction using graphene/polyvinylchloride nanocomposite coated fiber coupled to gas chromatography-flame ionization detector

- A graphene/polyvinylchloride nanocomposite was coated on a stainless steel.
- It was applied for headspace solid phase microextraction of phthalate esters.
- The analysis of the extracted phthalate esters was performed by GC-FID.
- Optimization of the extraction process was carried out using the response surface method.
- Good recoveries in real samples indicating the absence of matrix effects in the method.

In the current study, a graphene/polyvinylchloride nanocomposite was successfully coated on a stainless steel substrate by a simple dip coating process and used as a novel headspace solid phase microextraction (HS-SPME) fiber for the extraction of phthalate esters (PEs) from drinking water and edible vegetable oil samples. The prepared SPME fibers exhibited high extractability for PEs (due to the dominant role of π-π stacking interactions and hydrophobic effects) yielding good sensitivity and precision when followed by a gas chromatograph with a flame ionization detector (GC-FID). The optimization strategy of the extraction process was carried out using the response surface method based on a central composite design. The developed method gave a low limit of detection (0.06-0.08 μg L−1) and good linearity (0.2-100 μg L−1) for the determination of the PEs under the optimized conditions (extraction temperature, 70 ± 1 °C; extraction time, 35 min; salt concentration, 30% w/v; stirring rate, 900 rpm; desorption temperature, 230 °C; and desorption time, 4 min) whereas the repeatability and fiber-to-fiber reproducibility were in the range 6.1-7.8% and 8.9-10.2%, respectively. Finally, the proposed method was successfully applied to the analysis of PEs in drinking water and edible oil samples with good recoveries (87-112%) and satisfactory precisions (RSDs < 8.3%), indicating the absence of matrix effects in the proposed HS-SPME method.