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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

Orbifloxacin, European Pharmacopoeia (EP) Reference Standard
Supelco
Ampicillin, analytical standard
Sulfadimidine, European Pharmacopoeia (EP) Reference Standard
Sulfamethoxazole, European Pharmacopoeia (EP) Reference Standard
Sulfapyridine, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Ciprofloxacin, European Pharmacopoeia (EP) Reference Standard
USP
Sulfamethoxazole, United States Pharmacopeia (USP) Reference Standard
USP
Sulfadiazine, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Sodium phosphate dibasic, BioReagent, suitable for cell culture, suitable for insect cell culture, ≥99.0%, free-flowing, Redi-Dri
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, for chromatography
Sigma-Aldrich
Sodium phosphate dibasic, ≥99.5%
Sigma-Aldrich
Sodium phosphate dibasic, SAJ first grade, ≥99.0%
Sigma-Aldrich
Formic acid, SAJ first grade, 88.0-89.5%
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 300
Sigma-Aldrich
Acetonitrile, JIS special grade, ≥99.5%
Sigma-Aldrich
Acetonitrile, SAJ first grade, ≥99.0%
Sigma-Aldrich
Sodium phosphate monobasic, SAJ special grade, 99.0-101.0%
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
Sigma-Aldrich
Acetonitrile, for residue analysis, JIS 5000
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Formic acid, JIS special grade, ≥98.0%
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Sulfapyridine, VETRANAL®, analytical standard
Sigma-Aldrich
Ampicillin, anhydrous, 96.0-102.0% (anhydrous basis)
Sigma-Aldrich
Amoxicillin, 95.0-102.0% anhydrous basis
Supelco
Sulfapyridine, ≥99.0%