Determination of beta-agonist residues in bovine urine using liquid chromatography-tandem mass spectrometry.
A multiresidue method was developed and validated to screen bovine urine samples for 10 beta-2-adrenergic agonistic drugs--brombuterol, cimaterol, clenbuterol, clenpenterol, isoxsuprine, mabuterol, ractopamine, ritodrine, salbutamol, and tulobuterol--at the 2 microg/L level. The method is also quantitative in the range of 1 to 4 microg/L for all analytes except salbutamol. The procedure uses enzymatic digestion, liquid-liquid extraction, and cleanup on solid-phase extraction columns, followed by detection using a liquid chromatograph-tandem quadrupole mass spectrometer operated in the positive-ion atmospheric pressure chemical ionization multiple-reaction monitoring mode. Method validation included assessment of recoveries, repeatabilities, linearity of responses, decision limits, and detection capabilities. Overall average recoveries ranged from 70-91%; recoveries were generally lower for salbutamol. The decision limits ranged from 0.4-1.0 microg/L, and detection capabilities from 0.6-1.7 microg/L.
Dickson
Leslie C
LC
Centre for Veterinary Drug Residues, Canadian Food Inspection Agency, Saskatoon Laboratory, 116 Veterinary Rd, Saskatoon, SK S7N 2R3, Canada. dicksonl@inspection.gc.ca
MacNeil
James D
JD
Lee
Stephen
S
Fesser
Adrian C E
AC
D000318:Adrenergic beta-Agonists / Q000737:chemistry*; D000420:Albuterol / Q000032:analysis; D000814:Aniline Compounds / Q000032:analysis; D000818:Animals; D002138:Calibration; D002417:Cattle; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D002976:Clenbuterol / Q000031:analogs & derivatives* / Q000032:analysis; D004350:Drug Residues / Q000032:analysis; D004983:Ethanolamines / Q000032:analysis; D005561:Formates / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D005966:Glucuronidase / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D007477:Ions; D007556:Isoxsuprine / Q000032:analysis; D013058:Mass Spectrometry; D008956:Models, Chemical; D009584:Nitrogen / Q000737:chemistry; D010627:Phenethylamines / Q000032:analysis; D012312:Ritodrine / Q000032:analysis; D012680:Sensitivity and Specificity; D013726:Terbutaline / Q000031:analogs & derivatives* / Q000032:analysis
D000318:Adrenergic beta-Agonists; D000814:Aniline Compounds; D004983:Ethanolamines; D005561:Formates; D007477:Ions; D010627:Phenethylamines; C030544:formic acid; C107573:brombuterol; C060897:ractopamine; C010809:tulobuterol; D005966:Glucuronidase; D012312:Ritodrine; D009584:Nitrogen; D013726:Terbutaline; D000420:Albuterol; D007556:Isoxsuprine; C044573:mabuterol; D002976:Clenbuterol; C047411:cimaterol