In 1996, the European Union established provisional maximum residue limits (MRL) for gentamicin, neomycin, streptomycin and dihydrostreptomycin in milk and tissue (0.1-5 mg kg-1). For the detection of these four aminoglycosides, three enzyme linked immunosorbent assays (ELISA) for applications in milk and kidney were developed. The screening of defatted and diluted milk resulted in limits of determination (LDM) of < 0.01 mg l-1. Kidney samples were deproteinized with a trichloroacetic acid solution (3%) and after filtration and the addition of buffer, aliquots were used in the ELISA. The LDM of the four aminoglycosides in kidney were < 0.05 mg kg-1. The ELISA were found suitable for the semi-quantitative screening of milk and kidney for the presence of the four aminoglycosides far below the MRL levels. In randomly taken milk samples (n = 776) and in kidneys derived from healthy pigs (n = 124), the aminoglycoside residues found were far below their established MRL. In eight out of the 94 kidney samples obtained from diseased animals after emergency slaughter, aminoglycoside residues were above the MRL.

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The fate of ivermectin (IVM) residues was studied throughout the processing of daily bulk milk from 30 ewes (taken up to 33 d following subcutaneous administration of 0 . 2 mg IVM/kg b.w.) in the following milk products: yoghurt made from raw and pasteurized milk; cheese after pressing ; 30-and 60-day ripened cheese; and whey, secondary whey and whey proteins obtained after cheese-making (albumin cheese). The concentration of the H 2 B 1a component of IVM was analysed in these dairy products using an HPLC method with fluorescence detection. The mean recovery of the method was, depending on the matrix, between 87 and 100%. Limits of detection in the order of only 0 . 1 mg H 2 B 1a /kg of product were achieved. Maximum concentrations of IVM were detected mostly at 2 d after drug administration to the ewes. The highest concentration of IVM was found on day 2 in 60-day ripened cheese (96 mg H 2 B 1a /kg cheese). Secondary whey was the matrix with the lowest concentration of IVM (< 0 . 6 mg H 2 B 1a / kg). Residue levels fell below the limits of detection between day 5 (for secondary whey) and day 25 (for all cheese samples). In the matrices investigated, linear correlations between daily concentrations of IVM, milk fat and solid content were evident. During yoghurt production, fermentation and thermal stability of IVM was observed. During cheese production, approximately 35 % of the IVM, present in the raw (bulk) milk samples, was lost. From the results it was concluded that the processing of ewes' milk did not eliminate the drug residues under investigation. The consequences of IVM in the human diet were discussed. Milk from treated animals should be excluded from production of fat products like cheese for longer after treatment with IVM than for lower fat products.

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(1999) Suitability of the charm HVS and a microbiological multiplate system for detection of residues in raw milk at EU maximum residue levels, Veterinary Quarterly, 21:1, 21-27, DOI: 10.1080DOI: 10. /01652176.1999 Accepted for publication: October 13, 1998 SUMMARY In this paper we assessed the suitability of the Charm HVS and a newly developed microbiological multiplate system as post-screening tests to confirm the presence of residues in raw milk at or near the maximum permissible residue level (MRL). The multiplate system is composed of Bacillus stearothermophilus var. calidolactis plate at pH 8.0 for detection of beta-lactam antibiotics and tylosin, Bacillus cereus plate at pH 6.0 for detection of tetracyclines, Micrococcus luteus plate at pH 8.0 for detection of macrolides, Bacillus subtilis BGA plate at pH 8.0 for detection of aminoglycosides, trimethoprim-containing plate seeded with B. subtilis BGA at pH 7.0 for detection of sulphonamides, Escherichia coli plate at pH 6.0 for detection of quinolone and polymyxin, and Staphylococcus epidermidis plate at pH 6.0 for detection of novobiocin. For each test plate an action level is proposed in such a way that residues can be detected in raw bulk tank milk at levels near or below the established EU MRLs of beta-lactam antibiotics, tetracyclines, aminoglycosides, macrolides, sulphonamides, colistin, and quinolones. The Charm HVS test used to confirm the presence of tetracycline and macrolide residues gave false-positive results near the EU MRLs. The multiplate system gave valid results. Based on data for raw bulk tank milk samples and the proposed action level for each test plate for suspected samples, we demonstrated that the multiplate system is a reliable postscreening method that can be performed easily and cheaply in microbiological laboratories.