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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

Josamycin for peak identification, European Pharmacopoeia (EP) Reference Standard
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Ammonium acetate solution, 7.5 M
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Ammonium acetate solution, BioUltra, ~5 M in H2O
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Lincomycin hydrochloride, 96.0-102.0% (HPLC)
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Sodium phosphate monobasic monohydrate, BioXtra, ≥99.5% (T)
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Ammonium acetate solution, 50 % (w/v)
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Sodium hydroxide solution, 50% in H2O
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Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
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Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
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