Challenges on Production of a Certified Reference Material of Ochratoxin A in Roasted Coffee: A Brazilian Experience

• Published in: Journal of AOAC International 2019-11, Vol.102 (6), p.1725-1731
• Main Authors: do Rego, Eliane C P, Leal, Rodrigo V P, Bandeira, Raquel D C C, da Silva, Michelle R, Campos, Erika G, Petronilho, Caroline F, Rodrigues, Janaína M
• Format: Article
• Language: English
• ISSN: 1060-3271; 1944-7922
• DOI: 10.1093/jaoac/102.6.1725

Background: Coffee is an important agricultural commodity with technical barriers for exportation because of possible contamination with ochratoxin A (OTA), a mycotoxin nephrotoxic and carcinogenic. The maximum limit for OTA in roasted coffee is 5.0 μg/kg in the European Union and 10 μg/kg in Brazil, and the use of certified reference materials (CRM) is required for reliable measurements. Objective: This paper describes the development of a candidate CRM of OTA in roasted coffee following the requirements of ISO 17034 and ISO Guide 35. Methods: A primary method of isotope dilution MS was developed and validated using (13C20)-OTA as internal standard. The sample preparation was based on AOAC Official Methods of AnalysisSM using immunoaffinity column. Results: The linear working range is 2.0–15.0 μg/kg, with recoveries of 92.2–110.8% and relative SDs lower than 12.4%. The method was successfully applied to the feasibility study, which defined the procedure for preparation of a large batch around 5 μg/kg. It was produced by spiking blank roasted coffee with OTA standard, mixing and filling in amber flasks with 50 g of coffee, and storing at −80°C. The homogeneity study showed an acceptable degree of heterogeneity of 1.44%, and the short-term-stability study defined the conditions for transportation as maximum temperature of 50°C up to 28 days. Conclusions: These results show that certification is possible. Highlights: The long-term stability study at −20°C is in progress, and the characterization will be conduzed by a interlaboratory comparison. This material will be an important tool for QC in laboratories.