Development of analytical methods for multiresidue determination of quinolones in pig muscle samples by liquid chromatography with ultraviolet detection, liquid chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry.
ABSTRACT This paper presents a comparison between liquid chromatography with ultraviolet detection (LC-UV), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods developed for the multiresidue determination of 8 quinolones, around their maximum residue levels (MRLs) in pig muscle. The procedure involves common extraction of the quinolones from the tissues by traditional extraction, a step for clean-up and preconcentration of the analytes by solid-phase extraction (SPE) and a subsequent liquid chromatographic analysis. The methods present satisfactory results of linearity, precision and limits of quantification much lower than the MRLs established by the European Union for quinolones in pig tissues.
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Article: B. SAN MARTÍN, J. CORNEJO, D. IRAGÜEN, H. HIDALGO and A. ANADÓN (2007). Depletion study of Enrofloxacin and its metabolite Ciprofloxacin in edible tissues and feathers of white leghorn hens by liquid chromatography coupled tandem mass spectrometry. Journal of Food Protection 70 (8), 1952-1957.01/2007;
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ABSTRACT: The fragmentation and fragmentation behaviors of singly, doubly, and triply charged adducts of ciprofloxacin–poly(ethylene glycol) conjugate (P_Cf) with alkali metal ions, including Li+, Na+ and K+ ions, generated by electrospray (ESI) were studied as a function of collision energy. The product ion spectra of adducts with charge states +1, +2, and +3 are dominated by product ions arising from the loss-neutral moiety (ciprofloxacin) and CO2, and ions formed by dissociation of the precursor ion ([P_Cf + xM]x+) into product ions [P + (x − 1)M](x−1)+ and [Cf + M]+ (where P_Cf, P and Cf represent the ciprofloxacin–poly(ethylene glycol) conjugate, the poly(ethylene glycol) backbone without the endgroups, and the ciprofloxacin moiety, respectively; M is the alkali metal ion and x is the charge). It was found that the metal ions do not significantly alter the fragmentation pattern of ciprofloxacin–poly(ethylene glycol) conjugate. It is also interesting that the run and the shape of the survival yield curves for the singly and doubly charged adduct ions are independent of the cation. However, in the case of triply charged adducts, survival yield curves follow each other in the order K+, Na+, and Li+. Based on the experimental results, a fragmentation mechanism for the singly and multiply charged adducts of P_Cf with alkali metal ions is given. In addition, a tentative description of the signal intensity variations of the product ions with the lab frame collision energy is also reported.International Journal of Mass Spectrometry. 08/2008; 275(s 1–3):104–109.