title: A single laboratory-validated LC-MS method for the analysis of tulathromycin residues in bison and deer sera and selected tissues of white-tailed deer.
abstract: The performance characteristics of a newly developed liquid chromatography-mass spectrometry (LC-MS) method were validated and demonstrated to be fit for purpose in a pharmacokinetic and tissue depletion study of white-tailed deer and bison. Tulathromycin was extracted from bison and deer sera with acetonitrile or trifluoroacetic acid and K2 HPO4 (pH 6.8) buffer solution and cleaned up on a conditioned Bond-Elut cartridge. Tulathromycin, retained on the cartridge; it was eluted with methanol containing 2% formic acid, dried, re-constituted in methanol/1% formic acid, and analyzed by LC-MS. The limit of quantification (LOQ) of the method was 0.6 ng/mL in serum and 0.6 ng/g in tissue with RSDs ≤ 10% and accurate over the linear calibration range of 0.8-100 ng/mL for bison serum, 0.6-50 ng/mL for deer serum, 100-2500 ng/g for deer muscle tissue, and 500-5000 ng/g for deer lung tissue, all with coefficients of determination, r(2) ≥0.99. The validated method was used to quantify the concentration of tulathromycin residues in serum of bison and deer and selected tissue (lung and muscle tissue) samples obtained from 10 healthy, white-tailed deer that were administered the therapeutic dose approved for cattle (i.e., a single 2.5 mg/kg subcutaneous injection of tulathromycin in the neck). The deer were included in a tulathromycin drug depletion study. © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd.
authors.affiliation: CFIA Saskatoon Laboratory, Saskatoon, Canada.
authors.forename: Joe O
authors.initials: JO
authors.lastname: Boison
authors.affiliation: College of Pharmacy, School of Graduate Studies, University of Saskatchewan, Saskatoon, Canada.
authors.forename: Kali
authors.initials: K
authors.lastname: Bachtold
authors.affiliation: Western College of Veterinary Medicine, University of Saskatchewan, Saskatoon, Canada.
authors.forename: Johanna
authors.initials: J
authors.lastname: Matus
authors.affiliation: College of Pharmacy, School of Graduate Studies, University of Saskatchewan, Saskatoon, Canada.
authors.forename: Jane
authors.initials: J
authors.lastname: Alcorn
authors.affiliation: Western College of Veterinary Medicine, University of Saskatchewan, Saskatoon, Canada.
authors.forename: Murray
authors.initials: M
authors.lastname: Woodbury
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis / Q000097:blood / Q000493:pharmacokinetics*; D016164:Bison / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D003670:Deer / Q000097:blood*; D004187:Disaccharides / Q000032:analysis / Q000097:blood / Q000493:pharmacokinetics*; D004350:Drug Residues / Q000032:analysis / Q000493:pharmacokinetics*; D005260:Female; D006571:Heterocyclic Compounds / Q000032:analysis / Q000097:blood / Q000493:pharmacokinetics*; D057230:Limit of Detection; D008168:Lung / Q000378:metabolism; D009132:Muscles / Q000378:metabolism; D053719:Tandem Mass Spectrometry / Q000379:methods*; D019155:Veterinary Drugs / Q000032:analysis / Q000493:pharmacokinetics*; D018942:Macrolides
chemical_list: D000900:Anti-Bacterial Agents; D004187:Disaccharides; D006571:Heterocyclic Compounds; D019155:Veterinary Drugs; C485204:tulathromycin; D018942:Macrolides
keywords: LC-MS; bison and deer serum; deer lung and muscle tissue; depletion study; quantitative analysis; tulathromycin