关键词: 高效液相色谱-串联质谱法, 类固醇激素, 同位素内标法

Abstract: An analytical method for the determination of 4 steroid hormones in milk and milk power was developed by filtration solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry. Samples were extracted with acetonitrile, and purified on a PRiME HLB cartridge. Then the chromatographic separation was achieved using an Acquity BEH C18 column (2.1 mm × 100 mm, 2.5 μm) with a mobile phase consisting of water and acetonitrile. The compounds were ionized using an electrospray ionization source in the negative ion mode and quantitated by the internal standard method. The results showed that the calibration curves of all analytes had a good linear relationship in the concentration range of 0.2–100.0 ng/mL. The limits of detection and limits of quantitation were 0.4–2.0 and 0.8–4.0 μg/kg, respectively. The recoveries of the method were in range of 87.7%–110.8% with relative standard deviations (RSDs) of 0.85%–4.56% in milk and in range of 89.2%–107.4% with RSDs of 0.85%–4.56% in milk power. This method was proved to be rapid, sensitive, and useful for the quantification of 4 steroid hormones in milk and milk power samples.

Key words: high performance liquid chromatography-tandem mass spectrometry, steroid hormones, isotopic internal standard