A new multi-residue method for the analysis of sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine, sulfaguanidine and sulfamethoxazole) in non-target feeds using high-performance liquid chromatography-fluorescence detection (HPLC-FLD) and precolumnderivatization was developed and validated. Sulfonamides (SAs) were extracted from feed with an ethyl acetate/methanol/acetonitrile mixture. Clean-up was performed on a Strata-SCX cartridge. The HPLC separation was performed on a Zorbax Eclipse XDB C18 column with a gradient mobile phase system of acetic acid, methanol, and acetonitrile. The method was validated according to EU requirements (Commission Decision 2002/657/EC). Linearity, decision limit, detection capability, detection and quantification limits, recovery, precision, and selectivity were determined, and adequate results were obtained. Using the HPLC-FLD method, recoveries were satisfactory (79.3–114.0%), with repeatability and reproducibility in the range of 2.7–9.1% to 5.9–14.9%, respectively. Decision limit (CCα) and detection capability (CCβ) were 197.7–274.6 and 263.2–337.9 µg/kg, respectively, and limit of detection (LOD) and limit of quantification (LOQ) were 34.5–79.5 and 41.3–89.9 µg/kg, respectively, depending on the analyte. Results showed that this analytical procedure is simple, rapid, sensitive, and suitable for the routine control of feeds.
A liquid chromatography -diode array detector (HPLC-DAD) procedure has been developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), doxycycline (DC), enrofloxacin (ENR), ciprofloxacin (CIP), sarafloxacin (SAR) and flumequine (FLU) residues in animal drinking water. This method was applied to animal drinking water. Solid-phase extraction (SPE) clean-up on an Oasis HLB cartridge allowed an extract suitable for liquid chromatographic analysis to be obtained. Chromatographic separation was carried out on a C18 analytical column, using gradient elution with 0.1% trifluoroacetic acid -acetonitrile -methanol at 30 o C. The flow-rate was 0.7 mL/min and the eluate was analysed at 330 nm. The whole procedure was evaluated according to the requirements of the Commission Decision 2002/657/EC, determining specificity, decision limit (CCα), detection capacity (CCβ), limit of detection (LOD), limit of quantification (LOQ), precision and accuracy during validation of the method. The recoveries of TCs and FQs from spiked samples at the levels of 10, 100 and 1000 μg/L were higher than 82%. The developed method based on HPLC-DAD has been applied for the determination of four tetracyclines and four fluoroquinolones in animal drinking water samples.
The paper describes a microbiological method for the detection of antibacterial substances in feedingstuffs. The method allowed detection of the main antibiotic groups, including tetracyclines. In 2013-2014, a total of 171 feed samples were analysed to determine antibacterial substances. Among the analysed samples 84 (49.1%) were suspected to contain tetracyclines. Out of the 84 feeds analysed using chromatography, 28 (33.3%) contained undeclared tetracyclines, which were identified at concentrations ranging from 0.32 mg kg -1 to 48.98 mg kg -1 .
Tetracycline antibiotics, including tetracycline (TC), chlortetracycline (CTC), oxytetracycline (OTC) and doxycycline (DOX), are commonly used in veterinary medicine because of their broad-spectrum activity, cost effectiveness and certain favourable pharmacokinetic properties. The use of antibiotics in feed for non-medicinal purposes has been prohibited in the European Union. In Poland and other countries of the European Union, there are official national programmes for controlling the use of TCs and all other antibacterials in feed. This paper presents the pharmacological properties of TCs as well as the main reasons for and consequences of their use in feed. It also presents a chromatographic method for detection of TCs in animal feeds. The method is used in routine testing of food for the presence of tetracycline antibiotics. In the years 2015-2017, tetracycline antibiotics were detected in 31 out of 126 feed samples analysed by this method.
IntroductionThe authorisation of tylosin as feed additive was withdrawn for reasons of human health concerning resistance of pathogenic bacteria. An analytical method for the identification and quantification of tylosin in animal feed was developed and validated.Material and MethodsThe samples were extracted using an acidified methanol:water mixture and solid-phase extraction was employed for the isolation of the antibiotic from diluted feed samples. Tylosin was analysed by liquid chromatography with electrospray ionisation mass spectrometric detection. The method’s performance was evaluated in adherence to the Commission Decision 2002/657/EC.ResultsThe recovery of the analyte from spiked samples was determined to be in the range from 78.9% to 108.3% depending on tylosin concentrations. The CCα and CCβ values for tylosin in feeds were determined at 0.085 mg kg-1 and 0.091 mg kg-1, respectively. The method detection limit was found to be 0.035 mg kg-1 and the quantification limit 0.05 mg kg-1. The applicability of the developed method was tested by analysing real feed samples.ConclusionA reliable LC-MS method was developed to identify and quantify tylosin in animal feed with a good repeatability and a high specificity and sensitivity. Because of these characteristics, the proposed method is applicable and could be deemed necessary within the field of feed control and safety.
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