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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

Supelco
Sulfapyridine melting point standard, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
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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
Trimethoprim, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
USP
Erythromycin, United States Pharmacopeia (USP) Reference Standard
USP
Amoxicillin, United States Pharmacopeia (USP) Reference Standard
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Methanol, anhydrous, 99.8%
Sigma-Aldrich
Tetracycline, 98.0-102.0% (HPLC)
Sigma-Aldrich
Trimethoprim, ≥99.0% (HPLC)
Supelco
Acetic acid, analytical standard
Supelco
Sulfamethazine, VETRANAL®, analytical standard
Supelco
Methanol, analytical standard
Sigma-Aldrich
Erythromycin standard solution, 1 mg/mL in H2O
Supelco
Trimethoprim, VETRANAL®, analytical standard
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2,3-Diaminonaphthalene, BioReagent, suitable for fluorescence, ≥98.0% (HPLC)
Sigma-Aldrich
Erythromycin, tested according to Ph. Eur.
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Acetic acid, ≥99.5%, FCC, FG
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2,3-Diaminonaphthalene, ≥95% (HPLC), powder
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Tetracycline, 98.0-102.0% (HPLC)
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Sulfamethazine, 99.0-101.0% (on dried basis)
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Trimethoprim, ≥98.5%
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Ampicillin, meets USP testing specifications
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Erythromycin, meets USP testing specifications
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Sulfaguanidine
Sigma-Aldrich
Erythromycin, potency: ≥850 μg per mg