ABSTRACT
A method was developed and validated for determination and quantitation of tilmicosin residues in swine, cattle, and sheep edible tissues, as well as chicken fat, skin, and muscle over a concentration range of 0.025 microg/g-20 microg/g. For chicken kidney and liver, the method was validated over a range of 0.060 microg/g-20 microg/g. The tissue sample was extracted with methanol and a C18 cartridge was used for solid-phase extraction cleanup. A reversed-phase gradient liquid chromatographic method with detection at 280 nm was used to separate the tilmicosin from matrix components in 30 min run time. The limit of quantitation (LOQ) of the method was 0.025 microg/g for all tested tissues except chicken kidney and liver, for which the LOQ was 0.06 microg/g. Average recoveries for tissue samples ranged from 73 to 98%. Relative standard deviation values ranged from 0.6 to 14.7%.
Subject(s)
Anti-Bacterial Agents/analysis , Chickens , Chromatography, High Pressure Liquid/methods , Macrolides , Meat/analysis , Sheep , Swine , Tylosin/analogs & derivatives , Tylosin/analysis , Adipose Tissue/chemistry , Animals , Cattle , Drug Residues/analysis , Food Contamination , Kidney/chemistry , Liver/chemistry , Muscle, Skeletal/chemistry , Quality Control , Sensitivity and Specificity , Skin/chemistryABSTRACT
This method was developed and validated to detect and quantitate tilmicosin residues in cow milk over a range of 0.010-10 microg/mL, and in sheep milk over a range of 0.025-0.5 microg/mL. The procedure involves extracting the milk sample with acetonitrile and using a C18 cartridge to perform a solid-phase extraction cleanup of the extract. A reversed-phase gradient liquid chromatography method with detection at 280 nm is used to separate the tilmicosin from matrix components in a 30 min run time. The limit of quantitation of the method is 0.010 microg/mL for cow milk, and 0.025 microg/mL for sheep milk. Average percentage recoveries for milk samples ranged from 82 to 94%. Percentage relative standard deviation values ranged from 3.1 to 17.2%.
Subject(s)
Anti-Bacterial Agents/analysis , Chromatography, Liquid/methods , Macrolides , Milk/chemistry , Tylosin/analogs & derivatives , Animals , Cattle , Chromatography, Liquid/standards , Models, Chemical , Quality Control , Sensitivity and Specificity , Sheep , Specimen Handling , Tylosin/analysisABSTRACT
A capillary electrophoresis (CE) postcolumn radionuclide detector has been developed that uses a commercial phosphor-imaging detector and has been optimized for low-energy beta emitters. Eluant from the separation capillary is deposited on a membrane. Emission from radioactive analytes on the membrane is integrated using the phosphor-imaging system for 10-72 h. Results from the phosphor-imaging system are converted to conventional electropherograms. Modifications to a prior postcolumn CE deposition system have been accomplished by adding a buffer makeup capillary; this increases the electrolyte pH range and improves reproducibility. The limit of detection (LOD) for 35S-labeled analytes is 0.13 amol (8.7 pM or 0.007 Bq), while the LOD for 32P-labeled analytes is 4.9 zmol (0.33 pM or 0.002 Bq), with a linear range for 35S-Met from 1.5 amol to 1.5 fmol.
