Determination of Four Fluoroquinolones in Milk by Liquid Chromatography

Author:

Roybal José E1,Pfenning Allen P1,Turnipseed Sherri B1,Walker Calvin C1,Hurlbut Jeffrey A1

Affiliation:

1. U.S. Food and Drug Administration, Animal Drugs Research Center, Denver Federal Center, PO Box 25087, Denver, CO 80225-0087

Abstract

Abstract A liquid chromatographic (LC) method with fluorescence detection is presented for the analysis of 4 fluoroquinolones; enrofloxacin (ENRO), ciprofloxacin (CIPRO), sarafloxacin (SARA), and difloxacin (DIFLX) in milk. The procedure consists of extraction of milk with acidified ethanol, isolation and retention on a cation exchange solid-phase extraction column, elution with basic methanol, and LC analysis with fluorescence detection. LC analysis is performed by isocratic elution using an acetonitrile-2% acetic acid (15 + 85) mobile phase and an Inertsil phenyl column with fluorescence detection at excitation and emission wavelengths of 278 and 450 nm, respectively. A target level of 10 ppb for each of the 4 fluoroquinolones has been established for this method. Average recovery from fortified raw milk samples (5-100 ppb each) based on a 5-point standard curve calculation was 70-90%, with relative standard deviations of <15%.

Publisher

Oxford University Press (OUP)

Subject

Pharmacology,Agronomy and Crop Science,Environmental Chemistry,Food Science,Analytical Chemistry

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