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Development of a Method for the Analysis of Multiclass Antibiotic Residues in Milk Using QuEChERS and Liquid Chromatography-Tandem Mass Spectrometry.

Foodborne pathogens and disease (2015-08-11)
Yuan-long Wang, Zhen-min Liu, Jing Ren, Ben-heng Guo
ABSTRACT

A precise and simplified method of sample preparation for the simultaneous quantification of the antibiotics β-lactam, macrolide, tetracycline, sulfonamide, and quinolone in bovine milk was developed. The central composite design of response surface methodology was used to design and optimize the method for the determination of six different antibiotic residues in milk. The recovery of each antibiotic was studied using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Octadecylsilane (C18), primary secondary amine (PSA), and sodium acetate (Na acetate) were the main factors affecting the recovery of each antibiotic. After optimization, the maximum predicted recovery rate was 84.18% for erythromycin under the optimized conditions of 101.20 mg C18, 52.00 mg PSA, and 1.01 g Na acetate. The recovery rates of the five other antibiotic residues ranged from 86.09% to 115.99%. The results suggested that modified QuEChERS could effectively be implemented in the analysis of antibiotic residues in milk.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Tetracycline hydrochloride, powder, BioReagent, suitable for cell culture
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Formic acid, ≥95%, FCC, FG
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Acetonitrile, anhydrous, 99.8%
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Tetracycline hydrochloride, meets USP testing specifications
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Tetracycline hydrochloride, ≥95% (European Pharmacopoeia HPLC assay)
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Tetracycline hydrochloride, powder
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Ultrapure Acetonitrile, for DNA synthesis
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Acetonitrile, for DNA synthesis
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Acetonitrile, for DNA synthesis
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Ultrapure Acetonitrile
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Acetonitrile, electronic grade, 99.999% trace metals basis
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Acetonitrile
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Sodium sulfate, BioUltra, anhydrous, ≥99.0% (T)
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Erythromycin standard solution, 1 mg/mL in H2O
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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
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Sodium acetate, anhydrous, BioUltra, for luminescence, for molecular biology, ≥99.0% (NT)
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Sodium acetate solution, BioUltra, for molecular biology, ~3 M in H2O
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Sodium acetate, 99.995% trace metals basis
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Acetic acid, ≥99.5%, FCC, FG
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Sodium Acetate Anhydrous, >99%, FCC, FG
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Sodium sulfate, ≥99.99% trace metals basis
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Sodium sulfate, BioXtra, ≥99.0%
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Sodium acetate, powder, BioReagent, suitable for electrophoresis, suitable for cell culture, suitable for insect cell culture, ≥99%
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Sodium acetate, meets USP testing specifications, anhydrous
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Sodium acetate, BioXtra, ≥99.0%
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Sodium acetate, anhydrous, for molecular biology, ≥99%
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Erythromycin, potency: ≥850 μg per mg
Sigma-Aldrich
Erythromycin, BioReagent, suitable for cell culture