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 β-Lactam Residues

• Published in: Journal of agricultural and food chemistry 2006-07, Vol.54 (15), p.5267-5278
• Main Authors: Heller, David N, Nochetto, Cristina B, Rummel, Nathan G, Thomas, Michael H
• Format: Article
• Language: English
• Subjects: Animals; Anti-Bacterial Agents - analysis; antibiotic residues; antimicrobial agents; beta-lactam antibiotics; beta-Lactams - analysis; Biological and medical sciences; Chickens; Chromatography, Liquid - methods; drug residues; Drug Residues - analysis; Egg and egg product industries; eggs; Eggs - analysis; Female; fluoroquinolones; Fluoroquinolones - analysis; food contamination; Food industries; Fundamental and applied biological sciences. Psychology; liquid chromatography; mass spectrometry; multiresidue analysis; polar drug residues; quinolones; solid phase extraction; Spectrometry, Mass, Electrospray Ionization; sulfonamides; Sulfonamides - analysis; tetracyclines; Tetracyclines - analysis
• ISSN: 0021-8561; 1520-5118
• DOI: 10.1021/jf0605502

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 β-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 β-lactam drugs were not found by LC/MS/MS in eggs from hens dosed orally with β-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. Keywords: Residues in eggs; ion trap mass spectrometry; sulfonamide analysis; tetracycline analysis; fluoroquinolone analysis; β-lactam analysis; liquid chromatography/tandem mass spectrometry