Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

Abstract

A liquid chromatography -tandem mass spectrometry (LC-MS/MS) method for the determination of oxytetracycline (OTC), 4-epi oxytetracycline (4-epi OTC), tetracycline (TC), 4-epi tetracycline (4-epi TC), chlortetracycline (CTC), 4-epi chlortetracycline (4-epi CTC), doxycycline (DC), minocycline (MINO), methacycline (META) and rolitetracycline (ROLI) residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X) reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% -103.6%. The decision limits were from 109.0 to 119.8 µg/kg and detection capability varied within the range of 122.2 to 137.6 µg/kg, depending on the analyte.

Development, validation and application to real samples of a liquid chromatography with tandem mass spectrometry method for the determination of tetracyclines in beeswax

“…LC‐MS/MS has been presented as a sensitive technique for the determination of TCs in many complex biological samples, such as beeswax. The MS/MS settings previously described by our research team for the determination of TCs in muscle required optimization, because the LC‐MS system used in the presented method was different from that used before. The MS/MS parameters, like gas flow rates, source temperature conditions, and collision gas were adjusted to achieve maximum response for the instrument.…”

“…Polymeric columns were reported to reduce interaction of silanols and trace metals, but the results with a polymer column compared to a commonly used C8 or C18 bonded silica analytical column were less satisfactory . Many types of bonded silica analytical columns like Luna C18, Halo C18, Kinetex XB‐C18, and Nucleoshell RP 18 were tested in our previous study describing the determination of TCs in muscle . According to the findings of that research, the best results were achieved on the Luna C18 column and this column was selected for the separation of TCs and their isobaric epi forms in the presented study.…”

Assessment of various veterinary drug residues in animal originated food products

“…Of ten muscles were examined for Tet + residues where detection capability found in varied range between 122.2 and 137.6 µg/kg which depending on the analyte and the recoveries of all target compounds were 91.8-03.6%. The DL was measured between 109.0 and 119.8 µg [30]. Sopik et al [31] have developed and validated HPLC-MS/ MS multi residues method according to commission regulation 2002/657/EC to determine Tet + , Oxy-tet + hydrochloride, Chlor-tet + hydrochloride, and doxycycline hydrochloride with liquid-liquid extraction with trichloroacetic acid and McIlvaine buffer, followed by solid-phase extraction with HLB column was used to clean up the sample extract.…”

“…Of ten muscles were examined for Tet + residues where detection capability found in varied range between 122.2 and 137.6 μg/kg which depending on the analyte and the recoveries of all target compounds were 91.8-03.6%. The DL was measured between 109.0 and 119.8 μg [ 30 ]. Sopik et al .…”

Synthesis and evaluation of bisulfate/mesylate-conjugated chlortetracycline with high solubility and bioavailability

“…Therefore, it has been widely used in clinical applications to treat a variety of infectious microorganisms. TCs are usually used alone to treat diseases at therapeutic levels and promote animal growth and feed efficiency at subtherapeutic levels (4,5); additionally, the combination of probiotics could improve nursery pigs' performance, but there were no consistent benefits of feeding them either probiotics alone or in the combination with CTCs (6).…”