Novel IAC-LC-ESI-MS(2) analytical set-up for ochratoxin A determination in pork

A reliable exposure assessment of mycotoxin contamination relies on their unambiguous identification and accurate quantification. With such purpose, a new analytical methodology was developed for evaluation of ochratoxin A (OTA) contamination in pork. Briefly OTA extraction from minced muscle samples involved the use of acidified methanol, ultrasound treatment and centrifugation, followed by an immunoaffinity column (IAC) clean-up step before mass spectrometric detection (precursor-to-fragment transitions: m/z 404→m/z 358 and m/z 404→m/z 386) in positive ESI mode using SRM scanning. The method combines green chemistry principles (e.g. absence of highly toxic solvents commonly used in this matrix) with a validation according to the guidelines laid down by the 2002/657/EC European Decision parameters: recoveries varied between 98.5% and 100.6%, limits of detection (LOD) and quantification (LOQ) were estimated at 0.06 and 0.19 μg/kg, whereas decision limit (CCα) and detection capability (CCβ) were 0.01 and 0.50 μg/kg, respectively. The proposed analytical set-up was successfully applied to twenty pork samples commercially acquired.