Occurrence of PCDD/F, PCB, PBDE, PFAS, and organotin compounds in fish meal, fish oil and fish feed.

We analysed polychlorinated dibenzo-p-dioxins and furans (PCDD/F, dioxins), and polychlorinated biphenyls (PCB) in 13 fish meal, five fish oil, and seven fish feed samples. Polybrominated diphenyl ethers (PBDE), organotin compounds (OTC), and perfluoroalkylated substances (PFAS) were analysed in ten fish meal, two fish oil, and two fish feed samples. All measured TEQ concentrations of PCDD/F and PCB were below the maximum levels set by Directive 2002/32/EC. There was no correlation between concentrations of WHOPCDD/F-TEQ and indicator PCB in our samples. The most common congeners among PBDEs were BDE-47 and BDE-100. BDE-209 was present in five fish meals of the ten analysed. Tributyltin (TBT) was the predominant congener in all samples except in three fish meals, where monobutyltin (MBT) was the major congener. Perfluorooctane sulphonate (PFOS) was the predominant congener in six fish meals of the ten analysed. There was large variation in concentrations and congener distributions of the studied compounds between our samples. Our results underline a need to pay special attention to the origin and purity of feed raw material of marine origin.

A microbiological six-plate method for the identification of certain antibiotic groups in incurred kidney and muscle samples.

A microbiological method was developed for group level identification of antibiotics in incurred kidney and muscle samples from cattle and pigs. The method was composed of six test bacterium-plate growth medium combinations and the result was recorded as a profile of growth inhibition zones. The sample profiles were compared to two sets of references: one constructed with standard antibiotic solution profiles, and the other with these combined with profiles of microbiologically and chemically identified residues from incurred samples. The algorithm employed in profile comparison located the minimal sum of absolute pairwise differences over the tests, with the addition of a number of experimentally observed intra-test criteria. Chemical identification and quantitation of incurred residues was based on liquid chromatography. The method identified penicillin G as a penicillinase sensitive penicillin, enrofloxacin and ciprofloxacin belonging to fluoroquinolone group, and oxytetracycline belonging to tetracycline group. Each of these residues was microbiologically identified below the Maximum Residue Limit (MRL) for kidney tissue. Combining sample profiles with the standard reference data set did not enhance the resolution. Microbiological and chemical identification test results were in good agreement. The results of this study show that a microbiological identification method is a useful tool in preliminary characterisation of antibiotic residues in animal tissues.

Microbiological and chemical detection of incurred penicillin G, oxytetracycline, enrofloxacin and ciprofloxacin residues in bovine and porcine tissues.

Incurred penicillin G, oxytetracycline, enrofloxacin and ciprofloxacin residues in bovine and porcine muscle and kidney samples were analysed by microbiological and chemical methods, the former using Bacillus subtilis BGA as a test organism on agar media of pH 6, pH 7.2 and pH 8 and the latter using liquid chromatography. Least squares fits between the logarithms of the chemically obtained concentrations of the antimicrobials and the widths of the inhibition zones were used to estimate the inhibition zone widths corresponding to the maximum residue limit concentrations. In vitro sensitivities were determined with standard antimicrobial solutions. The results indicate that if B. subtilis BGA is used as a test organism, muscle tissue cannot be used as test material for screening oxytetracycline, enrofloxacin and ciprofloxacin residues on the plates used in this study, while penicillin G can be screened from muscle tissue. Because of the numerous factors causing or increasing variation in the analysis, the inhibition zone caused by a given antibiotic concentration cannot be predicted precisely. Therefore, a positive agar diffusion test needs to be confirmed chemically. If a kidney sample gives a positive agar diffusion test result, the antimicrobial concentration in a muscle sample from the same carcass should be checked chemically.