The determination of ß-agonist residues in bovine tissues using liquid chromatography-tandem mass spectrometry.

We aimed to develop a rapid, simple and reproducible method based on LC-tandem mass spectrometry (LC-MS/MS) to analyze ß-agonist residues (clenbuterol, zilpaterol, ractopamine and isoxsuprine) in bovine tissues. The method was validated in accordance with the European Council Decision 2002/657/EC. The samples were homogenized, and then 10 mL of an acetate buffer was added to a 5-g sample. The sample was then centrifuged at 12,000 rpm and filtered. Sodium hydroxide (2 m) was added to adjust pH of the sample that was centrifuged again. The extract was filtered through a solid-phase extraction column. The residue was re-dissolved in 250 µL acetonitrile and then subjected to LC-MS/MS. The separation was done on a C18 column. The mobile phase consisted of 0.1% formic acid in deionized water and 0.1% formic acid in methanol. The mean recoveries of ß-agonists were in the range of 84.3%-119.1% with relative standard deviations (%RSDs) of 0.683%-4.05%. Decision limits and detection capabilities of the analytes ranged from 0.0960 to 4.9349 µg/kg and from 0.0983 to 5.0715, respectively. This method was used to detect four ß-agonists in 100 bovine muscle, 100 liver and 100 kidney tissues from a slaughterhouse. No residue was found above the maximum residue limit level.

Determination of the Polychlorinated Biphenyls Distribution in Different Fat Tissues of Cattle by Age and Gender.

Polychlorinated biphenyls (PCBs), which cause environmental pollution, are found in animal-based fatty foods. Due to their long half-life and lipophilic properties, they can accumulate in the fat tissues of cattle. The study was conducted to compare the PCB levels (PCB28, 52, 101, 118, 138, 153, and 180) in the different fat tissues (muscle, liver, kidney, spinal cord, lung, back fat, perihepatic fat, and perirenal fat) of cattle by age and gender. This information is also useful to evaluate the exposure risks for different bovine edible tissues. Therefore, 15 female and 15 male cattle under 24 months of age and 15 female and 15 male cattle over 24 months of age were used, and 480 samples were analyzed for target PCBs using gas chromatography-mass spectrometry. Of all the samples, two (50.2 µg/kg in perihepatic fat and 51.1 µg/kg in kidney) were found above the maximum residue limit; these samples were taken from the animals in the elderly female group (over 24 months). There were more PCBs in cattle older than 2 years. Muscle, kidney, and perihepatic fat presented higher PCB concentrations than other tissues, and perirenal fat presented lower PCB concentrations than other tissues. PCB101, PCB153, and PCB138 were found to have the highest contribution to the PCB concentration. Thus, it is concluded that perihepatic fat, muscle, or kidney should be sampled, particularly in routine residue monitoring, and specifically analyzed for PCB101, PCB153, and PCB138.