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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

Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Sodium phosphate monobasic-16O4, 99.9 atom % 16O
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Erythromycin, Pharmaceutical Secondary Standard; Certified Reference Material
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Trimethoprim, ≥99.0% (HPLC)
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Erythromycin standard solution, 1 mg/mL in H2O
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Trimethoprim, VETRANAL®, analytical standard
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Erythromycin, tested according to Ph. Eur.
Millipore
Chlortetracycline Selective Supplement, suitable for microbiology
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Doxorubicin hydrochloride, suitable for fluorescence, 98.0-102.0% (HPLC)
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Sulfamethazine, 99.0-101.0% (on dried basis)
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Trimethoprim, ≥98.5%
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Doxorubicin hydrochloride, 98.0-102.0% (HPLC)
Sigma-Aldrich
Sulfamonomethoxine
USP
Erythromycin, United States Pharmacopeia (USP) Reference Standard
Doxorubicin hydrochloride, European Pharmacopoeia (EP) Reference Standard
Erythromycin, for microbiological assay, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
USP
Amoxicillin, United States Pharmacopeia (USP) Reference Standard
Marbofloxacin, European Pharmacopoeia (EP) Reference Standard
Trimethoprim, European Pharmacopoeia (EP) Reference Standard
Sulfaguanidine, European Pharmacopoeia (EP) Reference Standard
Enrofloxacin for system suitability, European Pharmacopoeia (EP) Reference Standard
USP
Doxorubicin hydrochloride, United States Pharmacopeia (USP) Reference Standard
USP
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Sulfaguanidine
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Supelco
Marbofloxacin, VETRANAL®, analytical standard
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Supelco
Phosphate Standard for IC, TraceCERT®, 1000 mg/L phosphate in water (nominal concentration)