Development of multiclass methods for drug residues in eggs: hydrophilic solid-phase extraction cleanup and liquid chromatography/tandem mass spectrometry analysis of tetracycline, fluoroquinolone, sulfonamide, and beta-lactam residues.
A method was developed for detection of a variety of polar drug residues in eggs via liquid chromatography/tandem mass spectrometry (LC/MS/MS) with electrospray ionization (ESI). A total of twenty-nine target analytes from four drug classes-sulfonamides, tetracyclines, fluoroquinolones, and beta-lactams-were extracted from eggs using a hydrophilic-lipophilic balance polymer solid-phase extraction (SPE) cartridge. The extraction technique was developed for use at a target concentration of 100 ng/mL (ppb), and it was applied to eggs containing incurred residues from dosed laying hens. The ESI source was tuned using a single, generic set of tuning parameters, and analytes were separated with a phenyl-bonded silica cartridge column using an LC gradient. In a related study, residues of beta-lactam drugs were not found by LC/MS/MS in eggs from hens dosed orally with beta-lactam drugs. LC/MS/MS performance was evaluated on two generations of ion trap mass spectrometers, and key operational parameters were identified for each instrument. The ion trap acquisition methods could be set up for screening (a single product ion) or confirmation (multiple product ions). The lower limit of detection for screening purposes was 10-50 ppb (sulfonamides), 10-20 ppb (fluoroquinolones), and 10-50 ppb (tetracyclines), depending on the drug, instrument, and acquisition method. Development of this method demonstrates the feasibility of generic SPE, LC, and MS conditions for multiclass LC/MS residue screening.
Heller
David N
DN
Center for Veterinary Medicine, U.S. Food and Drug Administration, Laurel, Maryland 20708, USA. david.heller@fda.hhs.gov
Nochetto
Cristina B
CB
Rummel
Nathan G
NG
Thomas
Michael H
MH
D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002645:Chickens; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D004531:Eggs / Q000032:analysis*; D005260:Female; D024841:Fluoroquinolones / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization; D013449:Sulfonamides / Q000032:analysis; D013754:Tetracyclines / Q000032:analysis; D047090:beta-Lactams / Q000032:analysis
D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D013449:Sulfonamides; D013754:Tetracyclines; D047090:beta-Lactams