Multi-residue analysis of tranquillizers in meat: confirmatory assays using mass spectrometry.

A rapid and sensitive multi-residue method was developed to attempt to confirm the presence of the beta-blocker carazolol and the tranquillizers acepromazine, azaperone, chlorpromazine, propionylpromazine and xylazine in pig muscle tissues. The procedure involves determination by liquid chromatography coupled with tandem mass spectrometry. The liquid chromatographic separation was performed on a Symmetry C18 column with gradient elution. A mixture of aqueous buffer, containing 0.01% m/v trifluoroacetic acid (pH 3.5), and acetonitrile at a flow rate of 0.4 ml min-1 was used as the mobile phase. The abundant parent ions [M+ H+] produced by positive electrospray ionisation were selected for collisional dissociation with argon. Fragment ions were recorded with daughter ion scan and multiple reaction monitoring. The analytes were identified unambiguously by assessing retention times and diagnostic ions in meat samples spiked from 50 micrograms kg-1 [maximum residue limit (MRL) for azaperone and azaperol] to 5 micrograms kg-1 (MRL for carazolol).

A one-plate microbiological screening test for antibiotic residue testing in kidney tissue and meat: an alternative to the EEC four-plate method?

A one-plate screening method is described for the microbiological detection of antibiotic residues by growth inhibition of Bacillus subtilis in agar medium, at pH 7, which contains trimethoprim for better detection of sulphonamides. beta-Glucuronidase is added to the samples to enable the detection of chloramphenicol residues. The sensitivity was determined for 16 antimicrobial substances frequently used in animal husbandry. A comparison was made with the sensitivity of the EEC four-plate test and existing maximum residue levels. The method has been used in Belgium for 5 years for the monitoring of antimicrobial residues in kidney tissue and meat of slaughter animals.

Immunoaffinity-chromatography purification of salbutamol in liver and HPLC-fluorometric detection at trace residue level.

A method combining immunoaffinity-chromatography (IAC) and high-performance liquid chromatography (HPLC) for the analysis of Salbutamol in liver with a low quantification limit of 1 micrograms/kg has been developed. Salbutamol was extracted with 0.01 mol/L HCl and purified by IAC. The samples were analysed on a liquid chromatograph fitted with a C18 mu-Bondapak column. A fluorometer was used for the detection of salbutamol. Recoveries of 67-80% could be obtained.