Determination of Ochratoxin A in wine at sub ng/mL levels by solid-phase microextraction coupled to liquid chromatography with fluorescence detection.
Solid-phase microextraction (SPME), using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber, interfaced with liquid chromatography-fluorescence detection (LC-FD) has been applied to the determination of Ochratoxin A (OTA) in wine samples. Compared to the most widely adopted extraction/clean-up procedure based on immunoaffinity columns (IAC), the solventless extraction is simpler and cost-effective, requiring the simple immersion of the fiber in diluted wine samples. Furthermore, a fast LC separation is achieved under isocratic conditions. The linear range investigated in wine was 0.25-8 ng/mL; at fortification levels of 0.5 and 2 ng/mL, within-day intra-laboratory precision (repeatability) values, expressed as RSD%, were 5.9 and 5.1, respectively, whereas between days (n = 4) precision was 8.5 and 7.1%, respectively. The limit of detection (LOD) at a signal-to-noise (S/N) ratio of 3 was 0.07 ng/mL; the limit of quantification (LOQ) calculated at S/N = 10 was 0.22 ng/mL, well below the European regulatory level of 2 ng/mL. The potential of the method has been demonstrated by the analysis of a number of different wine samples.
Aresta
Antonella
A
Dipartimento di Chimica, Università degli Studi di Bari, Via E. Orabona 4, 70126 Bari, Italy.
Vatinno
Rosa
R
Palmisano
Francesco
F
Zambonin
Carlo G
CG
D005591:Chemical Fractionation; D002853:Chromatography, Liquid / Q000379:methods*; D005453:Fluorescence; D005506:Food Contamination / Q000032:analysis; D006863:Hydrogen-Ion Concentration; D008832:Microchemistry; D009793:Ochratoxins / Q000032:analysis*; D014920:Wine / Q000032:analysis*
D009793:Ochratoxins; C025589:ochratoxin A