Validation of a high-performance liquid chromatography analytical method for ochratoxin A quantification in cocoa beans
Titel:
Validation of a high-performance liquid chromatography analytical method for ochratoxin A quantification in cocoa beans
Auteur:
Amezqueta, S. Gonzalez-Penas, E. Murillo, M. de Cerain, A. Lopez
Verschenen in:
Food additives and contaminants. Pt. A, Chemistry, analysis, control, exposure & risk assessment
Paginering:
Jaargang 21 (2004) nr. 11 pagina's 1096-1106
Jaar:
2004-11
Inhoud:
A validated high-performance liquid chromatography (HPLC) method with fluorescence detection for the quantitative analysis of ochratoxin A (OTA) in cocoa beans is described. OTA was extracted with methanol-3% sodium hydrogen carbonate solution and then purified with immunoaffinity columns before its analysis by HPLC. The validation of the analytical method was based on the following criteria: selectivity, linearity, limit of detection and quantification, precision (within- and between-day variability) and recovery, robustness and uncertainty. Detection and quantification limits were 0.04 and 0.1 μg kg-1, respectively. Recovery was 88.9% (relative standard deviation = 4.0%). This method was successfully applied to the measurement of 46 cocoa bean samples of different origins. A total of 63% of cocoa bean samples was contaminated with a level greater than the limit of detection. The means and medians obtained for cocoa bean were 1.71 and 1.12 μg kg-1, respectively. Surveillance controls should be set up in both crops and factories involved in transformation processes to avoid this mycotoxin in final products.