Two methods for measuring ochratoxin A in corn, oat, and grape juice were developed and compared. Flow injection (FI) and on-line liquid chromatography (LC) performances were evaluated separately, with both methods using a triple quadrupole tandem mass spectrometer (MS/MS) for quantitation. Samples were fortified with 13C uniformly labeled ochratoxin A as the internal standard (13C-IS) and prepared by dilution and filtration, followed by FI- and LC-MS/MS analysis. For the LC-MS/MS method, which had a 10 min run time/sample, recoveries of ochratoxin A fortified at 1, 5, 20, and 100 ppb in corn, oat, red grape juice, and white grape juice ranged from 100% to 117% with RSDs < 9%. The analysis time of the FI-MS/MS method was <60 s/sample, however, the method could not detect ochratoxin A at the lowest fortification concentration, 1 ppb, in all tested matrix sources. At 5, 20, and 100 ppb, recoveries by FI-MS/MS ranged from 79 to 117% with RSDs < 15%. The FI-MS/MS method also had ~5× higher solvent and matrix-dependent instrument detection limits (0.12–0.35 ppb) compared to the LC-MS/MS method (0.02–0.06 ppb). In the analysis of incurred corn and oat samples, both methods generated comparable results within ±20% of reference values, however, the FI-MS/MS method failed to determine ochratoxin A in two incurred wheat flour samples due to co-eluted interferences due to the lack of chromatographic separation.
Determination of Ochratoxin A Levels in Mixed Feed and Feed Stuffs Used in Some Laying Hens and Ruminant Enterprises of Sivas City
