title: Qualitative and Quantitative Drug residue analyses: Florfenicol in white-tailed deer (Odocoileus virginianus) and supermarket meat by liquid chromatography tandem-mass spectrometry.
abstract: A method for confirmation and detection of Florfenicol amine residues in white-tailed deer tissues was developed and validated in our laboratory. Tissue samples were extracted with ethyl acetate and cleaned up on sorbent (Chem-elut) cartridges. Liguid chromatography (LC) separation was achieved on a Zorbax Eclipse plus C18 column with gradient elution using a mobile phase composed of ammonium acetate in water and methanol at a flow rate of 300μL/min. Qualitative and quantitative analyses were carried out using liquid chromatography - heated electrospray ionization(HESI) and atmospheric pressure chemical ionization (APCI)-tandem mass spectrometry in the multiple reaction monitoring (MRM) interface. The limits of detection (LODs) for HESI and APCI probe were 1.8ng/g and 1.4ng/g respectively. Limits of quantitation (LOQs) for HESI and APCI probe were 5.8ng/g and 3.4ng/g respectively. Mean recovery values ranged from 79% to 111% for APCI and 30% to 60% for HESI. The validated method was used to determine white-tailed deer florfenicol tissue residue concentration 10-days after exposure. Florfenicol tissue residues concentration ranged from 0.4 to 0.6μg/g for liver and 0.02-0.05μg/g for muscle and a trace in blood samples. The concentration found in the tested edible tissues were lower than the maximum residual limit (MRL) values established by the federal drug administration (FDA) for bovine tissues. In summary, the resulting optimization procedures using the sensitivity of HESI and APCI probes in the determination of florfenicol in white-tailed deer tissue are the most compelling conclusions in this study, to the extent that we have applied this method in the evaluation of supermarket samples drug residue levels as a proof of principle.
authors.affiliation: Department of Environmental Toxicology, The Institute of Environmental and Human Health Texas Tech University, Lubbock, TX 79409-1163, United States.
authors.forename: Shanoy C
authors.initials: SC
authors.lastname: Anderson
authors.affiliation: Department of Environmental Toxicology, The Institute of Environmental and Human Health Texas Tech University, Lubbock, TX 79409-1163, United States.
authors.forename: Seenivasan
authors.initials: S
authors.lastname: Subbiah
authors.affiliation: Department of Environmental Toxicology, The Institute of Environmental and Human Health Texas Tech University, Lubbock, TX 79409-1163, United States.
authors.forename: Angella
authors.initials: A
authors.lastname: Gentles
authors.affiliation: Department of Environmental Toxicology, The Institute of Environmental and Human Health Texas Tech University, Lubbock, TX 79409-1163, United States.
authors.forename: Galen
authors.initials: G
authors.lastname: Austin
authors.affiliation: Department of Animal Care Services, Texas Tech University, Lubbock, TX 79409-3132, United States.
authors.forename: Paul
authors.initials: P
authors.lastname: Stonum
authors.affiliation: Department of Animal Care Services, Texas Tech University, Lubbock, TX 79409-3132, United States; Department of Animal and Food Sciences, Texas Tech University, Lubbock, TX 79409-2141, United States.
authors.forename: Tiffanie A
authors.initials: TA
authors.lastname: Brooks
authors.affiliation: Department of Animal and Food Sciences, Texas Tech University, Lubbock, TX 79409-2141, United States.
authors.forename: Chance
authors.initials: C
authors.lastname: Brooks
authors.affiliation: Department of Environmental Toxicology, The Institute of Environmental and Human Health Texas Tech University, Lubbock, TX 79409-1163, United States. Electronic address: ernest.smith@ttu.edu.
authors.forename: Ernest E
authors.initials: EE
authors.lastname: Smith
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis; D057230:Limit of Detection; D016014:Linear Models; D008460:Meat / Q000032:analysis*; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013839:Thiamphenicol / Q000031:analogs & derivatives* / Q000032:analysis
chemical_list: C035534:florfenicol; D013839:Thiamphenicol
keywords: Chromatography; Drug residue florfenicol amine; Florfenicol; LC–MS/MS; White-tailed deer