关键词: 水产品, 抗生素, 残留, 三重四极杆复合线性离子阱质谱, 筛查, 确证

Abstract: A rapid method for the screening and confirmation of 38 antibiotic residues in aquatic products was developed by high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (HPLC-Q-Trap-MS). The sample was extracted with acidified acetonitrile with EDTA-2Na, and then the extract was concentrated and degreased with n-hexane. Finally, the analytes were detected by HPLC-Q-Trap-MS in the multiple-reaction monitoring with information-dependent acquisition of enhanced product ion (sMRM-IDA-EPI) mode, followed by establishment of a multiple antibiotic database. The 38 antibiotics were confirmed by their retention times and ion pairs through database searching using the EPI library, and quantified by the internal standard method. All the antibiotics showed good linearity with correlation coefficients above 0.99. The limits of quantification (LOQs) for the antibiotics were in the range of 1.0–5.0 μg/kg. The average recoveries ranged from 63.5% to 117.3% with relative standard deviations of 2.6%–14.8% at spiked concentration levels of 1.0–50.0 μg/kg. The method is sensitive and accurate and can be successfully applied to the screening of antibiotic residues in aquatic products.

Key words: aquatic products, antibiotic, residues, triple quadrupole-linear ion trap mass spectrometry, screening, confirmation