Rapid determination of 54 pharmaceutical and personal care products in fish samples using microwave-assisted extraction—Hollow fiber—Liquid/solid phase microextraction

•Simultaneous enrichment and quantification of 54 trace PPCPs in fish samples.•A microextraction method combined synthetic SPME fiber with MAE and HF-LPME.•The microextraction method has low matrix interference and high EF for 54 PPCPs.•Using LC-HRMS as a quantification method for analysis of 54 trace PPCPs.•Develop a simple, rapid and solvent-less coupling technique. In this paper, a simple, rapid, solvent-less and environmental friendliness microextraction method, microwave-assisted extraction-hollow fiber-liquid/solid phase microextraction (MAE-HF-L/SME), was developed for simultaneous extraction and enrichment of 54 trace hydrophilic/lipophilic pharmaceutical and personal care products (PPCPs) from fish samples. A solid-phase extraction material, solid-phase microextraction (SPME) fiber, was synthesized. The SPME fiber had a homogeneous, loose structure and good mechanical properties, and they exhibited a good adsorption capacity for most PPCPs selected. The material formed the basis for the method of MAE-HF-L/SME. A method of liquid chromatography-high resolution mass spectroscopy (LC–HRMS) for analysis of 54 PPCPs. Under optimal synthesis and extraction conditions, the limits of detection (LODs, n=3) and the limits of quantitation (LOQs, n=10) for the 54 PPCPs were between 0.01–0.50μg·kg−1 and 0.052.00μg·kg−1, respectively. Percent recoveries and the relative standard deviations (RSDs) in spiked fish samples (n=6) were between 56.3%–119.9% and 0.3%–17.1%, respectively. The microextraction process of 54 PPCPs in MAE-HF-L/SME took approximately 12min. The method has a low matrix interference and high enrichment factor and may be applicable for determination of 54 different PPCPs in fish samples.