title: Validation of a high-performance liquid chromatography analytical method for ochratoxin A quantification in cocoa beans.
abstract: 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 mug 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 mug 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.
authors.affiliation: Organic and Pharmaceutical Chemistry Department, University of Navarra, E-31008 Pamplona, Spain.
authors.forename: S
authors.initials: S
authors.lastname: Amézqueta
authors.forename: E
authors.initials: E
authors.lastname: González-Peñas
authors.forename: M
authors.initials: M
authors.lastname: Murillo
authors.forename: A
authors.initials: A
authors.lastname: López de Cerain
mesh_terms: D002099:Cacao / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods; D005506:Food Contamination / Q000032:analysis*; D006801:Humans; D009183:Mycotoxins / Q000032:analysis; D009793:Ochratoxins / Q000032:analysis*; D015203:Reproducibility of Results
chemical_list: D009183:Mycotoxins; D009793:Ochratoxins; C025589:ochratoxin A