An
effective and efficient method for the determination of 18 β-agonists
in aquatic products using liquid chromatography tandem mass spectrometry
(LC-MS/MS) was successfully established. The method optimization was
conducted based on incurred samples to guarantee its practicability.
In this method, the sample was hydrolyzed with β-glucuronidase-arylsulfatase
in ammonium acetate solution and treated successively with protein
precipitation in 5% trichloroacetic acid in water, lipid removal with n-hexane, and further concentration and cleanup by solid-phase
extraction (hydrophilic–lipophilic balanced cartridge, primary–secondary
amine cartridge). Isotope-labeled internal standards and matrix-matched
calibration curves were used for quantification. The limit of quantification
(LOQ) was verified at 0.5–1.0 μg/kg (S/N > 10). This
method was evaluated with five different matrices, including eel,
roasted eel, pufferfish, shrimp, and crab, at 1×, 2×, and
10× LOQs, with good recoveries (>77%) and high replicate repeatability
(relative standard deviations (RSDs) <13%, intraday batch repeatability)
and further validated by three other accredited laboratories. A total
of 3 samples out of 37 tested aquatic products were found positive
for unknown incur sources (ractopamine, 0.38–2.1 μg/kg;
salbutamol 3.0 μg/kg; tulobuterol 2.9 μg/kg; clenbuterol
1.3 μg/kg; and clenpenterol, 0.3 μg/kg). The method has
demonstrated to be reliable, sensitive, and stable for multiresidue
screening of β-agonists for food safety monitoring.