An immunoaffinity column/HPLC procedure was developed to quantify low levels of ochratoxin A (OTA) in green coffee beans, roasted coffee beans, and soluble (instant) coffee with greater than 80% recoveries. The method was used to survey 116 soluble coffee samples from various countries and different manufacturers and showed contamination levels ranging from “not detectable” to 15.9 μg/kg. The highest levels of OTA were detected among soluble coffees that had been adulterated with coffee husks and/or coffee parchments (mean contamination level:  5.9 μg/kg). By comparison, OTA concentrations in pure soluble coffee samples were significantly lower, with a mean contamination level of 1.1 μg/kg. Although higher than normal figures have been found in some products purchased in East European countries, the results of this survey indicate that pure soluble coffee is not a major source of OTA in the diet, with estimated intakes being well within safety limits. Keywords: Ochratoxin A; soluble coffee; analysis; HPLC; adulteration

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As considerable inconsistencies are found in the literature regarding the influence of roasting and subsequent operations on the ochratoxin A (OTA) content of green coffee, experiments were undertaken to assess the evolution of OTA along an industrial soluble coffee manufacturing line. Both the variability and the amount of OTA naturally present in a lot of Thai Robusta green coffee were drastically reduced during soluble coffee manufacture. A small proportion of OTA was eliminated during green coffee cleaning, but the most significant reduction took place during roasting. The roast and ground coffee contained only 16% of the OTA originally present in the green coffee. Two phenomena are responsible for the elimination of OTA during roasting: a thermal degradation and a removal with chaff. Thermal degradation is the most important route of elimination, with <20% accounted for by the chaff. A further 20% reduction was observed during soluble coffee manufacture, so that the powder contained only 13% of the OTA initially present in the green beans.

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A collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for the determination of aflatoxin B1 and total aflatoxins at European regulatory limits. The test portion is extracted with methanol–water (8 + 2) for dried figs and paprika, and with methanol–water (8 + 2) plus hexane (or cyclohexane) for peanut butter and pistachios. The sample extract is filtered, diluted with phosphate buffer saline, and applied to an immunoaffinity column. The column is washed with water and the aflatoxins are eluted with methanol. Aflatoxins are quantitated by reversed-phase LC with post-column derivatization (PCD) involving bromination. PCD is achieved with either an electrochemical cell (Kobra cell) and addition of bromide to the mobile phase or pyridinium hydrobromide perbromide. Determination is by fluorescence. Peanut butter, pistachio paste, dried fig paste, and paprika powder samples, both naturally contaminated with aflatoxins and containing added aflatoxins, were sent to 16 collaborators in 16 European countries. Test portions of samples were spiked at levels of 2.4 and 9.6 ng/g for total aflatoxins which included 1.0 and 4.0 ng/g aflatoxin B1, respectively. Recoveries for total aflatoxins ranged from 71 to 92% with corresponding recoveries for aflatoxin B1 of 82 to 109%. Based on results for spiked samples (blind duplicates at 2 levels) as well as naturally contaminated samples (blind duplicates at 4 levels, including blank), the relative standard deviation for repeatability ranged from 4.6 to 23.3% for total aflatoxins and from 3.1 to 20.0% for aflatoxin B1. The relative standard deviation for reproducibility ranged from 14.1 to 34.2% for total aflatoxins, and from 9.1 to 32.2% for aflatoxin B1. The method showed acceptable within-laboratory and between-laboratory precision for all 4 matrixes, as evidenced by HORRAT values &lt;1, at the low levels of determination for both total aflatoxins and aflatoxin B1.