Skip to Content
Merck
  • 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

Supelco
Acetic acid, analytical standard
Supelco
Methanol, analytical standard
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Sigma-Aldrich
Doxorubicin hydrochloride, suitable for fluorescence, 98.0-102.0% (HPLC)
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Sodium phosphate monobasic-16O4, 99.9 atom % 16O
Sigma-Aldrich
Trimethoprim, ≥99.0% (HPLC)
Supelco
Trimethoprim, VETRANAL®, analytical standard
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Erythromycin standard solution, 1 mg/mL in H2O
Sigma-Aldrich
2,3-Diaminonaphthalene, BioReagent, suitable for fluorescence, ≥98.0% (HPLC)
Sigma-Aldrich
Erythromycin, tested according to Ph. Eur.
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Erythromycin, meets USP testing specifications
Sigma-Aldrich
Sulfamonomethoxine
Sigma-Aldrich
Erythromycin, potency: ≥850 μg per mg
Sigma-Aldrich
2,3-Diaminonaphthalene, ≥95% (HPLC), powder
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Sulfamethazine, 99.0-101.0% (on dried basis)
Sigma-Aldrich
Trimethoprim, ≥98.5%
Sigma-Aldrich
Sulfaguanidine
Sigma-Aldrich
Ampicillin, meets USP testing specifications
Erythromycin, for microbiological assay, European Pharmacopoeia (EP) Reference Standard
Doxorubicin hydrochloride, European Pharmacopoeia (EP) Reference Standard
Supelco
Sulfamonomethoxine, VETRANAL®, analytical standard
Supelco
Marbofloxacin, VETRANAL®, analytical standard
USP
Erythromycin, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C