Determination of p-Phenylphenol Residues in Vegetables and Fruits Based on Salting-out Homogeneous Liquid-liquid Extraction and High Performance Liquid Chromatography
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Abstract:
An analytical method was established to detect p-phenylphenol residues in vegetables and fruits by salting-out homogeneous liquid–liquid extraction (SHLLE) and high performance liquid chromatography (HPLC). Samples were extracted with acetonitrile and separated from sample solutions by salting out with sodium chloride. Separation was performed on a reversed phase C18-PFP column using methanol-water as the mobile phase for gradient elution, and the analyte was detected using a diode array/fluorescence dual detector and quantified by an external standard method. Key pre-treatment factors such as extraction solvent, extraction salt system, purification, concentration method and stability, and the influence of different chromatographic columns and mobile phase conditions on the separation effect were investigated and optimized. The results showed a strong linear relationship for p-phenylphenol between 0.05 and 100.00 µg/mL (diode array detector) and 0.01 and 5.00 µg/mL (fluorescence detector), with correlation coefficients (R2) all greater than 0.999. Limits of detection (LOD) of 0.03 mg/kg and 0.01 mg/kg were obtained for the diode array detector under ultraviolet and fluorescent conditions, respectively, with the limits of quantification (LOQ) reaching 0.10 mg/kg and 0.02 mg/kg. Average recoveries of 82.28%~110.7% and 85.83%~109.8% with relative standard deviations (RSD) of 2.60%~5.72% and 2.66%~5.26% were obtained under the three blank concentrations (LOQ, 2LOQ, and 10LOQ), respectively. This method is simple and fast, with good accuracy and reproducibility. Diode array/fluorescence dual detection is mutually qualitative, has good specificity, and is suitable for the determination of p-phenylphenol residues in vegetables and fruits.
