A method for the determination of 25 β-receptor agonist residues in milk and dairy products was established based on ultra-high performance liquid chromatography-tandem mass spectrometry. Samples were enzymatically hydrolyzed in 0.2 mol/L ammonium acetate solution at pH 5.2 for 16 h. After the removal of fat and protein through glass fiber filter paper, the filtrate was purified by solid phase extraction (SPE) using a PRiME MCX solid phase extraction column, and separated on a Waters BEH C18 column (100 mm × 2.1 mm, 1.7 μm) by gradient elution using a mobile phase composed of acetonitrile and 0.1% formic acid in water. Mass spectrometry was performed using an electrospray ionization source (ESI) in the positive ion mode with multiple reaction monitoring (MRM), and quantitative determination was performed using the internal standard method. The proposed method showed good linearity for all analytes in the concentration range of 0.2–50.0 ng/mL with coefficients of determination (R2) greater than 0.996; the recoveries ranged from 80.3% to 106.2% with relative standard deviations (RSDs) of 0.6%–8.5% (n = 6). The limits of detection (LOD) were 0.05–0.10 μg/kg, and the limits of quantification (LOQ) were 0.10–0.20 μg/kg. This method is simple, efficient and suitable for the determination of the 25 β-receptor agonist residues in milk and dairy products.

Using gas chromatography-tandem mass spectrometry (GC-MS), an indirect method was established for the simultaneous detection of 3-chloropropanol esters (3-MCPDE) and glycidyl esters (GE) in infant formula for special medical purposes. The conditions for sample extraction and transesterification/hydrolysis were optimized and stable isotope dilution was used to improve the accuracy and precision of the method. The results showed that the method exhibited good linearity in the range of 0.005–2.000 μg/mL (R2 ≥ 0.999), together with a limit of detection (LOD) of 5 μg/kg and a limit of quantification (LOQ) of 25 μg/kg (both calculated based on the corresponding amount of chloropropanol). The recoveries of the analytes spiked in infant formula for special medical purposes at 25, 125 and 250 μg/kg were 88.5%–104.1%, and the relative standard deviations (RSDs) for six replication determinations were less than 15% (n = 6). The levels of 3-MCPDE and GE in three types of commercial infant formula for special medical purposes were below the maximum limits set by the EU.