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  • Performance characterization of a quantitative liquid chromatography-tandem mass spectrometric method for 12 macrolide and lincosamide antibiotics in salmon, shrimp and tilapia.

Performance characterization of a quantitative liquid chromatography-tandem mass spectrometric method for 12 macrolide and lincosamide antibiotics in salmon, shrimp and tilapia.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-08-16)
Leslie C Dickson
ABSTRACT

This paper describes an extension and performance characterization of a quantitative confirmatory multi-residue liquid chromatography-tandem mass spectrometric method for residues of macrolide and lincosamide antibiotics, originally validated for application to bovine kidney tissues, to tissues of salmon, shrimp and tilapia. The 12 analytes include clindamycin, erythromycin A, gamithromycin, josamycin, lincomycin, neospiramycin 1, oleandomycin, pirlimycin, spiramycin 1, tildipirosin, tilmicosin and tylosin A. The limit of detection was 0.5 μg/kg. Within-laboratory precision evaluated over the analytical range of 5.0-50.0 μg/kg ranged from 4 to 17%. The accuracy of the method ranged from 80 to 112%. Recoveries ranged from 47 to 99% with all but one recovery above 60%. This is the first report of a quantitative confirmatory method for gamithromycin, pirlimycin and tildipirosin in fish and shrimp.

MATERIALS
Product Number
Brand
Product Description

Supelco
Lincomycin hydrochloride monohydrate, VETRANAL®, analytical standard
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Supelco
Phosphate Standard for IC, TraceCERT®, 1000 mg/L phosphate in water (nominal concentration)
Sigma-Aldrich
Lincomycin hydrochloride, 96.0-102.0% (HPLC)
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sigma-Aldrich
Josamycin, ≥90% (HPLC)
Sigma-Aldrich
Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
Sigma-Aldrich
Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Sigma-Aldrich
Lincomycin hydrochloride, BioReagent, suitable for cell culture
Sigma-Aldrich
Sodium phosphate monobasic monohydrate, BioReagent, suitable for electrophoresis, 98.0-102.0%
Sigma-Aldrich
Lincomycin hydrochloride, ≥90% (TLC)
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Sodium hydroxide, ultra dry, powder or crystals, 99.99% trace metals basis
Sigma-Aldrich
Sodium phosphate monobasic monohydrate, BioXtra, for molecular biology, ≥99.5% (T)
Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Supelco
Ammonium acetate, LiChropur, eluent additive for LC-MS
Sigma-Aldrich
Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
Sodium phosphate monobasic monohydrate, ACS reagent, ≥98%
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Sodium hydroxide solution, 50% in H2O
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Josamycin for peak identification, European Pharmacopoeia (EP) Reference Standard
Josamycin, European Pharmacopoeia (EP) Reference Standard