New magnetic oil palm fiber activated carbon-reinforced polypyrrole solid phase extraction combined with gas chromatography-electron capture detection for determination of organochlorine pesticides in water samples

Magnetic solid phase extraction (MSPE) employing oil-palm fiber activated carbon (OPAC) modified with magnetite (Fe3O4) and polypyrrole (OPAC-Fe3O4-PPy) was successfully used for the determination of two organochlorine pesticides (OCPs), namely endosulfan and dieldrin in environmental water samples. Analysis was performed using gas chromatography with micro-electron capture detection (GC-μECD). The effects of three preparation variables, namely Fe3O4:OPAC ratio, amount of pyrrole monomer, and amount of FeCl3 oxidant were optimized using Box-Behnken design (BBD) (R2 < 0.99, p-value < 0.001%). The optimum conditions were as follows: Fe3O4:OPAC ratio of 2:1 w/w, 1 g of FeCl3 and 100 μL of pyrrole monomer. The experimental results obtained agreed satisfactorily with the model prediction (> 90% agreement). Optimized OPAC-Fe3O4-PPy composite was characterized using field emission scanning electron microscope, vibrating sample magnetometer and Fourier transform infrared spectroscopy. Four numerical parameters of MSPE procedure was optimized using BBD. The significance of the MSPE parameters were salt addition > sample solution pH > extraction time and desorption time. Under the optimized conditions (extraction time: 90 s, desorption time: 10 min, salt: 0%, and pH: 5.8), the method demonstrated good linearity (25-1000 ng L-1) with coefficients of determination, R2 > 0.991, and low detection limits for both endosulfan (7.3 ng L-1) and dieldrin (8.6 ng L-1). The method showed high analyte recoveries in the range of 98.6-103.5% for environmental water samples. The proposed OPAC-Fe3O4-PPy MSPE method offered good features such as sustainability, simplicity, and rapid extraction.