High-performance liquid chromatographic determination of ochratoxin A in artificially contaminated cocoa beans using automated sample clean-up.
A HPLC method is described for the analysis of ochratoxin A at low-ppb levels in samples of artificially contaminated cocoa beans. The samples are extracted in a mixture of methanol-water containing ascorbic acid, adjusted to pH and evaporated to dryness. Samples in this state are then placed onto a Benchmate sample preparation workstation where C18 solid-phase extraction operations are performed. The resulting materials are evaporated to dryness and analyzed by reversed-phase HPLC with fluorescence detection. The method was evaluated for accuracy and precision with R.S.D.s for multiple injections of sample and standard calculated to 1.1% and 2.5% for sample and standard, respectively. Recoveries of ochratoxin A added to cocoa beans ranged from 87-106% over the range of the assay.
Analytical Service, Hershey Foods Technical Center, PA 17033, USA.
W J
WJ
Hurst
R A
RA
Martin
D001322:Autoanalysis; D002099:Cacao / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents; D009183:Mycotoxins / Q000032:analysis*; D009793:Ochratoxins / Q000032:analysis*; D013050:Spectrometry, Fluorescence
D007202:Indicators and Reagents; D009183:Mycotoxins; D009793:Ochratoxins; C025589:ochratoxin A