Determination of icariside, hyperoside and psoralen in food by liquid chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was built to determine icarside, hyperoside and psoralen in food. The samples were extracted with 70% methanol, the solid and semi-solid hotpot seasoning samples were purified by solid phase extraction column, and then determined by HPLC-MS/MS. Acetonitrile and 0.1% formic acid solution were used as the mobile phase, and the gradient elution was adopted for analysis. As shown in the results, the analytes had good linearity in the range of 0.05−100 ng/mL, and the correlation coeffificients (R²) were greater than 0.999. In this method, the limits of quantitation (LOQ) of psoralen, icariside and hyperoside in liquid samples were 1.25, 25.0 and 12.5 μg/L respectively; while the LOQs of psoralen, icariside and hyperoside in solid samples and hotpot seasoning samples were 1.25, 25.0 and 12.5 μg/kg, respectively. The liquid beverage, solid beverage, health food (in the form of oral liquid, capsule, tablet), integrated alcoholic beverage and solid hotpot seasoning were selected as representative samples and used for method validation. The average spiked recoveries at 3 levels (LOQ, 2 LOQ, 10 LOQ) were in the range of 83.7%−115.0%, and the relative standard deviations were in range of 0.5%−9.4% (n = 6). The method is rapid, accurate and sensitive, which is suitable for the simultaneous determination of icariside, hyperoside and psoralen in different food matrices.