A new method for the analysis of four target flavonoids in two kinds of citrus samples by ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed. Main variables affecting the UHPSFC separation were optimized, and under the optimized conditions the four target compounds (tangeretin, nobiletin, hesperetin and naringenin) can be separated within 10 min. The UHPSFC method allowed the determination of the four target compounds in the diluted stock solutions with limit of detection (LOD) ranging from 1.08 to 2.28 μg mL⁻¹, and limit of quantification (LOQ) ranging from 1.45 to 4.52 μg mL⁻¹, respectively. The coefficients of determination (R2) of the calibration curves were higher than 0.9950. The recoveries of the four target compounds at three different concentrations were in the range of 82.4–117.6%. The validation results demonstrated that the proposed method is simple, accurate, time-saving and environment friendly, and it is applicable to a variety of complex samples such as medicine-food dual purpose herbs and functional foods.
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