Determination of Ochratoxin A in Black and White Pepper, Nutmeg, Spice Mix, Cocoa and Drinking Chocolate by High-Performance Liquid Chromatography Coupled with Fluorescence Detection: Collaborative Study

A method validation study for the determination of ochratoxin A in black and white pepper (Piper spp.), nutmeg (Myristica fragrans), spice mix (blend of ginger, turmeric, pepper, nutmeg and chili), cocoa powder and drinking chocolate was conducted according to the "International Harmonized Protocol" of the International Union of Pure and Applied Chemistry. The method is based on the extraction of samples with aqueous methanol, followed by a cleanup of the extract with an immunoaffinity column. The determination is carried out by RP-LC coupled with a fluorescence detector. The study involved 25 participants representing a cross-section of research, private, and official control laboratories from 12 EU Member States together with Turkey and Macedonia. Mean recoveries for spices ranged from 71 to 85% and for cocoa and drinking chocolate from 85 to 88%. The RSD for repeatability (RSDr) for spices ranged from 5.6 to 16.7% and for cocoa and drinking chocolate from 4.5 to 18.7%. The RSD for reproducibility (RSDR) ranged from 9.5 to 22.6% for spices and from 13.7 to 30.7% for cocoa and drinking chocolate. The resulting HorRat for spices ranged from 0.4 to 1 and for cocoa and drinking chocolate from 0.6 to 1.4 according to the Horwitz function modified by Thompson. The method showed acceptable within-laboratory and between-laboratory precision for each matrix, and it conforms to requirements set by current EU legislation.

CUBERO LEON Elena;  BOUTEN Katrien;  SENYUVA Hamide;  STROKA Joerg; 

2017-05-03

AOAC INT

JRC105011

1060-3271,   

https://publications.jrc.ec.europa.eu/repository/handle/JRC105011,   

10.5740/jaoacint.16-0430,