Determination of Benzo[a]pyrene in Edible Oil by Nano Rod-Like MgO Based Solid Phase Extraction Combined with High Performance Liquid Chromatography-Fluorescence Detection
In this study,a rod-like MgO nanomaterial was synthesized by a direct precipitation method,and a method for the rapid analysis of BaP content in edible oil was established by combining rod-like MgO based solid phase extraction(SPE)and high-performance liquid chromatography with fluorescence detection(HPLC-FLD).The synthesized rod-like MgO was characterized by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),scanning electron microscopy(SEM),specific surface area and pore size analyser.The results showed that the MgO nanomaterials were polycrystalline cubic structure with rod-like morphology and large specific surface area.The average pore size of MgO nanomaterials is 11.0 nm,and the BET specific surface area is 102.4 m2·g-1.The large specific surface area provides abundant action sites with target analytes when used as SPE sorbent.In order to obtain high extraction efficiency of BaP,some key SPE factors including the adsorbent dosage,the type of washing solution,the type and volume of eluent,and the volume of the sample solution were optimized in detail.The optimal conditions were as follows:100 mg MgO nanomaterial,7 mL 0.1 g/mL oil in n-hexane as loading solution,ethyl acetate as cleaning solvent,and 3 mL of dichloromethane containing 3％methylimidazole as eluent.Under the optimized conditions,the linear range of BaP in edible oil was 0.5-20.0 μg/kg with the determination coefficient of the linear equation(R2)of 0.9999,and the limits of detection(LOD)and quantification(LOQ)of the method calculated at three and ten times of the signal-to-noise ratio(S/N ratio)were 0.10 μg/kg and 0.33 μg/kg,respectively.Meanwhile,the recoveries of BaP at the low,medium and high spiked concentrations were between 85.3％and 96.9％in edible oil,and the relative standard deviations(RSDs)of the intra-day and inter-day were in the range of 2.3％-9.0％,indicating satisfactory precision and accuracy.Finally,the method was applied to the analysis of BaP in eight actual oil samples,and,the recoveries ranged from 77.8％to 92.5％with the RSDs less than 9.8％,which indicated that the method has good application potential in the analysis of real samples.
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