title: Validated LC-MS-MS Method for Simultaneous Analysis of 17 Barbiturates in Horse Plasma for Doping Control.
abstract: A rapid and sensitive method for simultaneous screening, quantification and confirmation of 17 barbiturates in horse plasma using liquid chromatography-tandem mass spectrometry is described. Analytes were recovered from plasma by liquid-liquid extraction using methyl tert-butyl ether, separated on a C18 column, and analyzed in negative electrospray ionization mode. Multiple-reaction monitoring was employed for screening and quantification. Confirmation for the presence of the analytes was achieved by comparing ion intensity ratio. The ranges for limits of detection, quantification and confirmation were 0.003-1 ng/mL (S/N ≥ 3), 0.01-2.5 ng/mL and 0.02-5 ng/mL, respectively. The linear dynamic range of the method was 0.1-100 ng/mL. The precision and accuracy at 0.5, 5 and 50 ng/mL of all 17 barbiturates during intra-day assay were 1.6-8.6% and 96-106%, respectively. For inter-day assay, precision and accuracy at the same three concentrations were 2.6-8.9% and 96-106%, respectively. Analysis of all 17 analytes was completed within 7 min. Thus, the present method is fast, simple, sensitive and reproducibly reliable.
authors.affiliation: Department of Clinical Studies, University of Pennsylvania School of Veterinary Medicine, New Bolton Center Campus, 382 West Street Road, Kennett Square, PA 19348, USA.|National Institute for Food and Drug Control, No. 2 Tiantanxili, Beijing 100050, China.
authors.forename: Ying
authors.initials: Y
authors.lastname: Liu
authors.affiliation: United States Equestrian Federation, Equine Drug Testing & Research Center, 1509 Bull Lea Rd, Lexington, KY 45011, USA.
authors.forename: Cornelius E
authors.initials: CE
authors.lastname: Uboh
authors.affiliation: Department of Clinical Studies, University of Pennsylvania School of Veterinary Medicine, New Bolton Center Campus, 382 West Street Road, Kennett Square, PA 19348, USA.
authors.forename: Xiaoqing
authors.initials: X
authors.lastname: Li
authors.affiliation: Department of Clinical Studies, University of Pennsylvania School of Veterinary Medicine, New Bolton Center Campus, 382 West Street Road, Kennett Square, PA 19348, USA.
authors.forename: Fuyu
authors.initials: F
authors.lastname: Guan
authors.affiliation: Department of Clinical Studies, University of Pennsylvania School of Veterinary Medicine, New Bolton Center Campus, 382 West Street Road, Kennett Square, PA 19348, USA.
authors.forename: Youwen
authors.initials: Y
authors.lastname: You
authors.affiliation: New York Drug Testing & Research Program, New York State University at Morrisville, 777 Warren Rd, Ithaca, NY 14850, USA.
authors.forename: George A
authors.initials: GA
authors.lastname: Maylin
authors.affiliation: Chinese Pharmaceutical Association, No. 9 SOHO Building, Beijing 100022, China.
authors.forename: Fengchang
authors.initials: F
authors.lastname: Zhu
authors.affiliation: Department of Clinical Studies, University of Pennsylvania School of Veterinary Medicine, New Bolton Center Campus, 382 West Street Road, Kennett Square, PA 19348, USA.
authors.forename: Lawrence R
authors.initials: LR
authors.lastname: Soma
mesh_terms: D000818:Animals; D001463:Barbiturates / Q000097:blood*; D004300:Doping in Sports; D006736:Horses; D059625:Liquid-Liquid Extraction; D008738:Methyl Ethers; D010949:Plasma; D015813:Substance Abuse Detection / Q000379:methods*
chemical_list: D001463:Barbiturates; D008738:Methyl Ethers; C043243:methyl tert-butyl ether