Two different clean-up procedures for liquid chromatographic determination of ochratoxin A in urine.
This paper describes two different procedures for extraction of ochratoxin A (OTA) from urine samples: one using acidic chloroform-methanol mixture, followed by solid-phase extraction (SPE) clean-up and the other using commercial Chem Elut columns and a chloroform-formic acid mixture. The recovery of OTA using the procedure with silica gel columns was 82% with a R.S.D. < 8.4% and the detection and quantitation limits were 0.5 and 1.5 ng OTA/ml, respectively. The recovery of OTA in the second procedure with urine samples purified only on commercial Chem Elut columns was 95% with R.S.D. < 4.0%, and detection and quantitation limits 0.3 and 0.9 ng/ml, respectively. Both procedures of OTA extraction effectively eliminate interfering substances and give reliable and repeatable results. However, the procedure with Chem Elut columns gave higher recovery and lower detection and quantitation limits. It was successfully applied in determining OTA in human urine samples.
Domijan
Ana-Marija
AM
Unit of Toxicology, Institute for Medical Research and Occupational Health, Ksaverska c. 2, 10000, Zagreb, Croatia. adomijan@imi.hr
Peraica
Maja
M
Miletić-Medved
Marica
M
Lucić
Ana
A
Fuchs
Radovan
R
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D009793:Ochratoxins / Q000652:urine*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence
D009793:Ochratoxins; C025589:ochratoxin A