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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

Clindamycin hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Sodium phosphate dibasic, BioReagent, suitable for cell culture, suitable for insect cell culture, ≥99.0%, free-flowing, Redi-Dri
Sigma-Aldrich
Sodium phosphate dibasic, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, E 339, anhydrous, 98-100.5% (calc. to the dried substance)
USP
Lincomycin hydrochloride, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Sodium phosphate dibasic, puriss. p.a., ACS reagent, anhydrous, ≥99.0% (T)
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Lincomycin hydrochloride for system suitability, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Sodium phosphate dibasic, ACS reagent, ≥99.0%
Sigma-Aldrich
Sodium hydroxide-16O solution, 20 wt. % in H216O, 99.9 atom % 16O
Sigma-Aldrich
Poly(tetrafluoroethylene), powder, 200 μm particle size
Lincomycin hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Clindamycin hydrochloride, United States Pharmacopeia (USP) Reference Standard
Supelco
Clindamycin hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Poly(tetrafluoroethylene), powder, ≥350 μm particle size
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Poly(tetrafluoroethylene), powder (free-flowing), 1 μm particle size
Sigma-Aldrich
Sodium phosphate dibasic, 99.95% trace metals basis
Sigma-Aldrich
Poly(tetrafluoroethylene), powder, 35 μm particle size
Sigma-Aldrich
Poly(tetrafluoroethylene), powder (free-flowing), ≤12 μm particle size
Sigma-Aldrich
Clindamycin hydrochloride, lincosamide antibiotic
Sigma-Aldrich
Sodium phosphate dibasic, ReagentPlus®, ≥99.0%
Sigma-Aldrich
Sodium phosphate dibasic, BioReagent, suitable for cell culture, suitable for insect cell culture, ≥99.0%
Sigma-Aldrich
Sodium phosphate dibasic, for molecular biology, ≥98.5% (titration)
Sigma-Aldrich
Sodium phosphate dibasic, BioXtra, ≥99.0%
Sigma-Aldrich
Sodium phosphate dibasic, BioUltra, for molecular biology, ≥99.5% (T)
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O