Restricted access supramolecular solvents for the simultaneous extraction and cleanup of ochratoxin A in spices subjected to EU regulation

A simple and high-throughput sample treatment, based on the use of a supramolecular solvent with restricted access properties (SUPRAS-RAM), was developed for the quantification of ochratoxin A (OTA) in spices subjected to EU regulation. The RAM properties of the SUPRAS permitted exclusion of macromolecules by chemical and physical mechanisms, and pigments and essential oils did not influence OTA extraction. Sample treatment took 10 min and required minute amounts of spice (0.2 g) and volume of SUPRAS (0.4 mL). After sample centrifugation, the crude extracts were directed analyzed by liquid chromatography/fluorescence detection (LC-FD) using external calibration. Method validation proved that it met the performance criteria set by the EU guidelines in terms of sensitivity, recoveries, precision, selectivity and trueness. Recoveries found for OTA in spices classified as difficult and unique commodities by the EU (i.e. Capsicum, Piper nutmeg, ginger and turmeric) ranged from 81 to 101%, with repeatability and intermediate precision, expressed as relative standard deviation, in the intervals 0.4-7% and 2-9%, respectively. Method detection and quantification methods were 1.2 and 3 μg/kg. The method meets the requirements to be applied in enforcement and surveillance programs related to OTA in spices.