Optimization of dispersive liquid-phase microextraction based on solidified floating organic drop combined with high-performance liquid chromatography for the analysis of glucocorticoid residues in food

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Abstract

A rapid, simple, cost-effective dispersive liquid-phase microextraction based on solidified floating organic drop (SFOD-LPME) was developed in this study. Along with high-performance liquid chromatography, we used the developed approach to determine and enrich trace amounts of four glucocorticoids, namely, prednisone, betamethasone, dexamethasone, and cortisone acetate, in animal-derived food. We also investigated and optimized several important parameters that influenced the extraction efficiency of SFOD-LPME. These parameters include the extractant species, volumes of extraction and dispersant solvents, sodium chloride addition, sample pH, extraction time and temperature, and stirring rate. Under optimum experimental conditions, the calibration graph exhibited linearity over the range of 1.2–200.0 ng/ml for the four analytes, with a reasonable linearity(r2: 0.9990–0.9999). The enrichment factor was 142–276, and the detection limits was 0.39–0.46 ng/ml (0.078–0.23 μg/kg). This method was successfully applied to analyze actual food samples, and good spiked recoveries of over 81.5%–114.3% were obtained.

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