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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, European Pharmacopoeia (EP) Reference Standard
Josamycin for peak identification, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Ammonium acetate solution, 7.5 M
Sigma-Aldrich
Lincomycin hydrochloride, ≥90% (TLC)
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, 96.0-102.0% (HPLC)
Sigma-Aldrich
Ammonium acetate solution, BioUltra, ~5 M in H2O
Sigma-Aldrich
Sodium phosphate monobasic monohydrate, BioXtra, ≥99.5% (T)
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Ammonium acetate solution, 50 % (w/v)
Sigma-Aldrich
Josamycin, ≥90% (HPLC)
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, powder
Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Sigma-Aldrich
Sodium hydroxide, BioUltra, ≥98.0% (T), pellets
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, reag. Ph. Eur., K ≤0.02%, ≥98%, pellets
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Sigma-Aldrich
Sodium hydroxide, reagent grade, ≥98%, pellets (anhydrous)
Sigma-Aldrich
Sodium hydroxide, ACS reagent, ≥97.0%, pellets
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Sodium hydroxide solution, 5.0 M
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Sodium hydroxide solution, 50% in H2O
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Sodium hydroxide, pellets, semiconductor grade, 99.99% trace metals basis
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Sodium hydroxide, reagent grade, 97%, flakes
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Sodium hydroxide, beads, 16-60 mesh, reagent grade, 97%
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Sodium hydroxide solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Sodium hydroxide solution, 0.2 M