Development and validation of a method for the analysis of tetracyclines in chicken-muscle by liquid chromatography-electrospray-mass spectrometry in tandem (LC-ESI-MS/MS)

Abstract

Recebido em 20/12/09; aceito em 8/7/10; publicado na web em 9/11/10 A LC-ESI-MS/MS method was developed and validated according to the European Union decision 2002/657/EC, for the determination of tetracyclines (TCs) in chicken-muscle since Europe is one of the main markets for Brazilian products. Linearity of r > 0.9979, limits of quantification in the range of 7.0-35.0 ng/g, average recoveries of 89.38 -106.27%, within-day and betweenday precision were adequate for all TCs. The decision limit and the detection capability were 93.00-106.46 ng/g and 95.84-114.38 ng/g, respectively. This method is suitable for application in surveillance programmes of residues of TCs in chicken-muscle samples.

Concurrent Determination of Tigecycline, Tetracyclines and Their 4-Epimer Derivatives in Chicken Muscle Isolated from a Reversed-Phase Chromatography System Using Tandem Mass Spectrometry

“…Therefore, methanol was used to dissolve the standard in the preparation of the stock solution, a slightly acidic solvent was used as the diluent in the preparation of the working solution, and trichloroacetic acid was used in both diluent and mobile phase B to reduce possible solvent interference. Acidified protein precipitants (methanol and acetonitrile) [ 41 , 42 , 47 , 49 ] and buffer solution [ 43 , 44 , 45 , 46 , 48 , 50 ] were used as extractants, and acidifiers included formic acid, acetic acid, trifluoroacetic acid and EDTA. EDTA was used as the extractant in this study to minimize the chelation of tetracyclines with metal cations in biological samples while maintaining the freeness of the targets [ 41 ].…”

“…The analytes in this study included four tetracyclines (TC, CTC, OTC and DOXY), as specified in China’s current national food safety standards, coupled with their three 4-epimer derivatives (4-epi-TC, 4-epi-CTC and 4-epi-OTC) and the novel glycylcycline (TGC). Of the studies where HPLC–MS/MS was used as the detection method, some studies [ 41 , 42 , 43 , 44 , 45 , 46 ] investigated a range of analytes that was not as comprehensive as that used in the present study. The analytes involved in the study by Nakazawa et al [ 48 ] included demeclocycline but did not contain 4-epimer derivatives or TGC.…”

“…To avoid isomerization and degradation, slightly acidic solvents were used in the LC separation of tetracyclines, such as formic acid [ 41 , 42 , 43 , 44 , 45 ], oxalic acid [ 43 , 46 , 47 , 48 , 49 ] and malonic acid [ 50 ]. In the study published by Tölgyesi et al, a LC–MS/MS method and a LC–DAD method were established, and formic acid and oxalic acid were used in the mobile phase, respectively [ 43 ].…”

LC-MS/MS methodology development and validation for the screening and quantification of five antibiotics in water

“…For this, a mixed standard was injected 10 times with a signal-tonoise ratio of at least 10. 21,45,46 2.8.4 Precision and accuracy. Precision (repeatability) and accuracy of the method were determined using QC intra-day and inter-day (three days) with ve replicates at 3 concentration levels, namely, 10, 100 and 200 ng mL À1 .…”