TITLE

Cryogenic grinding pre-treatment improves extraction efficiency of fluoroquinolones for HPLC-MS/MS determination in animal tissue

AUTHOR(S)
Lolo, Manuel; Pedreira, Sandra; Váquez, Beatriz I.; Franco, Carlos M.; Cepeda, Alberto; Fente, Cristina A.
PUB. DATE
March 2007
SOURCE
Analytical & Bioanalytical Chemistry;Mar2007, Vol. 387 Issue 5, p1933
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
An efficiency extraction of fluoroquinolones in chicken muscle was achieved by pulverizing it in a freezer mill before treatment with NaOH (10mM)/MeCN (1:1). The improvement of cryogenic grinding in the extraction was demonstrated for the same piece (whole leg) of four chickens treated with enrofloxacin in equal doses. A confirmatory method based on high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used to analyze the extracts. The chromatographic separation was achieved in 5min with a Synergi Fusion-RP 80A (50 x 2mm, 4μm) column filled with a hybrid polymer. The HPLC was coupled with a detector based in a quadrupole–linear ion trap Q-TRAP that allows a confirmatory detection according to the European legislation. The specificity of the method was assessed by testing a number of representative blank muscle samples ( n = 10) to verify the absence of potential interfering compounds. The limits of detection and quantitation were 2 and 5ng g­1 of quinolones in muscle samples, respectively. The chromatographic method was demonstrated to be linear for the range studied (5–500ng g­1) with the P value for lack-of-fit in the ANOVA table greater or equal to 0.10 (calibration coefficient 0.9998 and 0.9996 for ciprofloxacin and enrofloxacin, respectively). The mean intra-day relative standard deviation (RSD) ( n = 6, c = 50ng g­1) was 6%; inter-day assay gave a RSD of 12%. The extraction and clean-up were carried out in one step with very satisfactory recovery data (between 65 and 101%).
ACCESSION #
24109137

 

Related Articles

Share

Read the Article

Courtesy of THE LIBRARY OF VIRGINIA

Sorry, but this item is not currently available from your library.

Try another library?
Sign out of this library

Other Topics