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  • Simultaneous determination of 38 veterinary antibiotic residues in raw milk by UPLC-MS/MS.

Simultaneous determination of 38 veterinary antibiotic residues in raw milk by UPLC-MS/MS.

Food chemistry (2015-03-22)
R W Han, N Zheng, Z N Yu, J Wang, X M Xu, X Y Qu, S L Li, Y D Zhang, J Q Wang
ABSTRACT

A selective and rapid method has been developed to determine, simultaneously, 38 veterinary antibiotic residues in raw milk by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). One milliliter of raw milk was diluted with 0.5 mL water and 3 mL acetonitrile, then purified using an Oasis HLB cartridge. The eluates were evaporated by nitrogen drying and then reconstituted to 4 mL with water/acetonitrile (8:1) before being injected into the UPLC-MS/MS system. The results indicated recoveries of 68-118% for 14 β-lactams, 79-118% for eight quinolones, 71-106% for eight sulfonamides, 76-116% for four tetracyclines, 78-106% for three macrolides, and 88-103% for one lincosamides, with coefficients of variation less than 15% for intraday and interday precisions. The limit of quantification for all antibiotics was 0.03-10 μg kg(-1). This methodology was then applied to field-collected real raw milk samples and trace levels of four antibiotics were detected.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Sodium phosphate monobasic-16O4, 99.9 atom % 16O
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Erythromycin, BioReagent, suitable for cell culture
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Doxorubicin hydrochloride, 98.0-102.0% (HPLC)
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Ampicillin, meets USP testing specifications
Sigma-Aldrich
Sulfamonomethoxine
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Doxorubicin hydrochloride, suitable for fluorescence, 98.0-102.0% (HPLC)
Sigma-Aldrich
Sulfamethazine, 99.0-101.0% (on dried basis)
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Trimethoprim, ≥98.5%
Sigma-Aldrich
Acetic acid, suitable for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Erythromycin standard solution, 1 mg/mL in H2O
Millipore
Chlortetracycline Selective Supplement, suitable for microbiology
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Trimethoprim, ≥99.0% (HPLC)
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Erythromycin, tested according to Ph. Eur.
Sigma-Aldrich
2,3-Diaminonaphthalene, BioReagent, suitable for fluorescence, ≥98.0% (HPLC)
Sigma-Aldrich
Erythromycin, meets USP testing specifications
Sigma-Aldrich
Sulfaguanidine
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Supelco
Trimethoprim, VETRANAL®, analytical standard
Supelco
Acetic acid, analytical standard
Supelco
Methanol, analytical standard
Doxorubicin hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
Erythromycin, for microbiological assay, European Pharmacopoeia (EP) Reference Standard