Abstract: A method based on ultra performance convergence chromatography-tandem mass spectrometry (UPCC-MS/MS) with pass-through solid phase extraction was established for the determination of 19 sex hormones in health foods. The samples were extracted with methanol containing 1% formic acid, and the extract was purified by solid phase extraction using PRiME HLB columns. The chromatographic separation was achieved on a UPCC Torus 2-PIC column (3.0 mm × 100 mm, 1.7 μm) under gradient elution using a mobile phase composed of supercritical carbon dioxide and methanol containing 0.1% formic acid. The separated compounds were analyzed by tandem MS with an electrospray ionization (ESI) source in the positive/negative alternate mode using multiple reaction monitoring. Ninety-seven percent methanol containing 0.2% formic acid and 98% aqueous acetonitrile containing 0.2% ammonia water were used as the auxiliary pump mobile phases. The external standard method was used to quantitatively analyze the sex hormones in sample solutions. Good linear relationship was obtained between the peak area and concentration in the tested concentration ranges (R2 ≥ 0.997 1). The limits of detection and limits of quantification were 0.03?0.85 (RSN = 3) and 0.10?2.5 μg/kg (RSN =10), respectively. The average recoveries (n = 9) at three spiked levels were in the range of 77.8%?111.7% with relative standard deviations (RSDs) between 1.1% and 8.4%. The developed method was successfully used for the determination of actual samples. This method is fast, simple, specific, environmentally friendly and suitable to determine the contents of sex hormones in health foods.

Key words: pass-through solid phase extraction; ultra performance convergence chromatography-tandem mass spectrometry; sex hormones; health foods