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

Sigma-Aldrich
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, for residue analysis
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Methanol, SAJ special grade
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Phosphate Standard for IC, TraceCERT®, 1000 mg/L phosphate in water (nominal concentration)
Doxorubicin hydrochloride, European Pharmacopoeia (EP) Reference Standard
Supelco
Marbofloxacin, VETRANAL®, analytical standard
USP
Erythromycin, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Trimethoprim, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Sulfapyridine melting point standard, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Supelco
Erythromycin, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Sigma-Aldrich
Erythromycin, tested according to Ph. Eur.
Supelco
Sulfamonomethoxine, VETRANAL®, analytical standard
Erythromycin, for microbiological assay, European Pharmacopoeia (EP) Reference Standard
USP
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
USP
Amoxicillin, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Supelco
Trimethoprim, VETRANAL®, analytical standard
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
2,3-Diaminonaphthalene, BioReagent, suitable for fluorescence, ≥98.0% (HPLC)
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)