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Determination of Ochratoxin A in wine at sub ng/mL levels by solid-phase microextraction coupled to liquid chromatography with fluorescence detection.

Aresta A, Vatinno R, Palmisano F, Zambonin CG

Dipartimento di Chimica, Università degli Studi di Bari, Via E. Orabona 4, 70126 Bari, Italy.

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.

Published 1 May 2006 in J Chromatogr A, 1115(1): 196-201.
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