RESUMEN
Antibiotic drug residues are crucial to ensure food safety and minimize risk to human health. Herein, a sensitive high-performance liquid chromatography−tandem mass spectrometry (HPLC−MS/MS) method was developed and validated for the determination of antibiotic residues (mainly amphenicols) consisting of chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF), and florfenicol amine (FFA) in aquatic products. Amphenicols were well separated on a Kinetex F5 (100 mm × 3.0 mm, 2.6 µm) chromatographic column with the mobile phases of 1 mM ammonium acetate aqueous solution and methanol solution and measured after positive and negative electrospray ionizations using four internal standards. To our knowledge, it was the first time to report the good performance of F5 column and four internal standards for the determination of amphenicols. The established method featured a good linear relationship between chromatographic peak area ratios and the concentrations of amphenicols (R2 > 0.992), a wide and low detection matrix-based range of 0.01−5 µg/L, a low detection limit of 0.01 µg/kg, etc. The spiked assays evidenced the accuracy and reliability of the developed method with the recoveries between 84.0 and 105%, the intraday relative standard deviations (RSDs) over the range of 0.769−13.7%, and the interday RSDs over the range of 0.582−13.3%. Finally, the proposed method was applied to investigate amphenicol residues in various aquatic products, including fish, shrimp, crab, shellfish, and other aquatic species.
RESUMEN
Tetrodotoxin (TTX) was simultaneously detected in the fresh and heat-processed aquatic products by high-performance liquid chromatography-tandem mass spectrometry method. The detection conditions were investigated, including the chromatography column and mobile phase. Based on the optimized parameters, a sensitive determination method of TTX was established. The proposed method featured the merits of a good linear relationship between signal and TTX concentration (R2 = 0.9998), a wide detection matrix-based range of 0.2-100 ng/g, and a low detection limit of 0.2 ng/g, etc. The spiked assays evidenced its accuracy and reliability with recoveries of 90.5-107.2%. Finally, the developed method was simultaneously successfully applied in the determination of TTX in various fresh and heat-processed aquatic products.
