食物与营养失调杂志

Development of a High- Performance Liquid Chromatography with Diode- Array Detection Method using Monolithic Column for Simultaneous Determination of Five Tetracyclines Residues in Fish Muscles

Ibtissem Ghorbel-Abid, Habibi Belhassen, Rim Lahsini, Dalila Chehimi Ben Hassen and Malika Trabelsi-Ayadi

Development of a High- Performance Liquid Chromatography with Diode- Array Detection Method using Monolithic Column for Simultaneous Determination of Five Tetracyclines Residues in Fish Muscles

A simple and accurate high performance liquid chromatography with diode array detection method was developed and validated for simultaneous determination of residues of five tetracyclines in fish muscles. Chromatographic separation was achieved in 14 min using a monolithic column, monitoring was at 355 nm and the mobile phase was consisting of oxalic acid, acetonitrile and methanol. Samples were extracted and purified using solid phase extraction cartridge with mean recoveries ranged from 72.1% to 92.2%. The current method was validated and applied on fish muscle in aquaculture according to the commission decision criteria 2002/657/EC. Samples spiked at different concentration levels (0.5, 1 and 1.5 times the maximum residue limit) were analyzed. It is demonstrated that the new method is robust for detection and quantitative determination of tetracyclines residues. Decision limit (CCα) ranged from 117 to 128 μg Kg-1 and capacity of detection (CCβ) from 118 to 154 μg Kg-1.

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