Foreword: mycotoxins in a changing world

This special issue arose because of the changes in the global landscape in relation to the impact and implications of our changing climate on food security and quality, consumer habits, trade and economics, regulations and scientific thinking. The EU green paper (EC, 2007) on climate change (CC) has suggested significant hot spots in different regions where food production will be considerably affected both in quality and quantity. Indeed, a recent UNEP report on ‘Emerging Issues of Environmental Concern’ (UNEP, 2016) has included a section entitled ‘Poisoned chalice: Toxin accumulation in crops in an era of climate change’ which refers to the impact that aflatoxin contamination is having in low and middle income countries (LMICs)

Certified reference materials for testing of mycotoxins

This factsheet summarises the CRMs from JRC-IRMM for testing of mycotoxinsJRC.D-Institute for Reference Materials and Measurements (Geel

Report on the 2011 Proficiency Test of the European Union Reference Laboratory for Mycotoxins, for the Network of National Reference Laboratories: Determination of aflatoxin B1 in baby food, maize powder, animal feed and test solution

This report presents the results of a proficiency test of the EU-RL for Mycotoxins which focused on the determination of aflatoxin B1 in food and feed samples. Sixty nine participants from 28 countries registered for the exercise. Sixty-one sets of results were reported for the solution, 58 for the baby food, 67 for the maize powder and 62 for the animal feed. One laboratory did not report any results. In total about 90% of the attributed z scores were below an absolute value of two, which indicated that most of the participants performed satisfactory or better.JRC.D.5-Food Safety and Qualit

Report on the 2014 Proficiency Test of the European Union Reference Laboratory for Mycotoxins, for the Network of National Reference Laboratories - Determination of Aflatoxin B1 in Copra (Coconut powder)

This report presents the results of the PT of the EURL for Mycotoxins which focused on the determination of aflatoxin B1 (Afla B1) in coconut powder samples. Sixty-one participants from 31 countries registered for the exercise and fifty-eight sets of results were reported. Only z-scores were used for an evaluation of performance. In total 91 % of the attributed z scores were below an absolute value of two, which indicated that most of the participants performed satisfactorily.JRC.D.5-Standards for Food Bioscienc

Report on the 2008 Proficiency Test of the Community Reference Laboratory for Mycotoxins, for the Network of National Reference Laboratories, regarding the Determination of Deoxynivalenol in a Cereal Product and a Test Solution

A proficiency test was conducted by the Community Reference Laboratory for Mycotoxins with 33 European National Reference Laboratories (NRLs) for Mycotoxins and 2 Laboratory from candidate countries, thus a total of 35 participants. Test materials were a deoxynivalenol (DON) solution in acetonitrile and three cereal test materials. Laboratories determined the DON content by either enzyme linked immuno sorbent assay (ELISA), gas chromatography (GC) or reverse-phase high-performance liquid-chromatography (RP-HPLC). One NRL did not report any results. Applying the Horwitz equation as a basis for the target standard deviation (19% in the case of this proficiency test), 27 out of the remaining 34 laboratories reported values within the z-score limit of 2 after recovery correction of the result for the DON-positive sample. Twenty-five laboratories reported results within a z-score limit of 1. Thus, 79 % of the participating laboratories performed satisfactorily in the proficiency test. No z scores were calculated for the blank material.JRC.D.8-Food safety and qualit

REPORT OF THE FOLLOW-UP COLLABORATIVE STUDY Determination of the sum of Fumonisin B1 and B2 in Compound Animal Feed and Maize by Immunoaffinity Column Clean-up and High Performance Liquid Chromatography with Fluorometric Detection

The accurate determination of mycotoxins in food and feed matrices for which EU legislative limits apply require robust and reliable analytical techniques. The robustness and reliability are best shown through validation by a collaborative study. Previous collaborative studies dealing with other mycotoxins have shown that it is possible to achieve performance characteristics which are fit-for-purpose provided suitable methodology is available. As with any interlaboratory comparison homogeneity between the test units is of utmost importance. Due to the complexity of food and feed matrices particular care has to be taken during test material preparation to achieve this. Methods for the determination of Fumonisin B1 (FB1) and Fumonisin B2 (FB2) have been subject to a collaborative study in the past and the methodology used involved immunoaffinity clean-up to purify the sample extracts. Detection was afforded by derivatisation of the Fumonisins to yield fluorescent derivatives before a chromatographic separation. The reagent used was o-phtaldialdehyde and mercaptoethanol. However, pre-column derivatisation does have disadvantages related to more demanding chromatography and the instability of the derivatives. Strict time control of all processes is required to obtain adequate repeatability which necessitates the use of programmable auto liquid samplers (ALS). This may be circumvented by using post column derivatisation instead. Here the native Fumonisins are separated and reagents are added constantly to the effluent of the chromatographic column. An additional pump, a mixing Tee, and additional tubing are needed for post column derivatisation replacing the need for a sophisticated ALS. During method development it could be shown that both methods can perform equally well with respect to the requirements by EU legislation for method performance and working range. A collaborative study to validate a method for the "Determination of Fumonisin B1 and B2 in Baby Food, Breakfast Cereals and Animal Feed by Immunoaffinity Column Clean-up with High Performance Liquid Chromatography and Fluorometric Detection" failed partially because of problems with the immunoaffinity columns (IAC) used for the study. After modifications to the method protocol regarding a check of proper performance of the IAC and the sample extract clean-up we describe below the results of a repeat of the study for compound animal feed and maize.JRC.D.8-Food safety and qualit

Report on the 2007 Proficiency Test of the Community Reference Laboratory Network - Determination of Aflatoxins in a Peanut Product and a Test Solution

A proficiency test was conducted with 31 European National Reference Laboratories (NRLs) for mycotoxins and one Laboratory from a candidate country. Test materials were a mixed aflatoxin (Af) solution in acetonitrile and two candidate Certified Reference Materials (CRM) - one "aflatoxin positive" and one "blank" material - that have not yet been released. Laboratories determined the aflatoxin content by reverse-phase high-performance liquid-chromatography (RP-HPLC) with either fluorescence or mass-selective detection against their own standard solutions as reference. Applying the modified Horwitz equation according to Thompson as a basis for the target standard deviation (22% in the case of this proficiency test), 26 out of 32 laboratories achieved z scores of less than 2 and 17 laboratories reported values within the uncertainty range for both aflatoxin B1 and total aflatoxins in the candidate CRM after correction for recovery in both cases.JRC.D.8-Food safety and qualit

2014 Proficiency Test of the European Union Reference Laboratory for Mycotoxins for the Network of National Reference Laboratories - Determination of Zearalenone in Maize Oil

This report presents the results of the PT of the EURL for Mycotoxins which focused on the determination of zearalenone in maize oil. Forty-eight participants from thirty countries (among them 32 NRLs, 2 Non-EU Reference Laboratories and 13 official food control laboratories) registered for the exercise and 46 sets (Sample A and B) of results were reported. Only z-scores were used for the evaluation whether an individual laboratory underperformed. In total, 87 % of the attributed z scores were below an absolute value of two, which indicates that most of the participants performed satisfactorily.JRC.D.5-Standards for Food Bioscienc

Report on the 2007 Proficiency Test for the Determination of Ochratoxin A in Capsicum ssp (Paprika Powder)

A proficiency test was conducted with 68 laboratories from 17 EU Member States and four Third Countries. Test materials were one naturally contaminated "Ochratoxin A positive" and one "Ochratoxin A blank" capsicum material. The majority of laboratories chose to determine the ochratoxin A content by reverse-phase high-performance liquid-chromatography (RP-HPLC) with fluorescence detection against their own standard solutions as reference. Applying the modified Horwitz equation according to Thompson as a basis for the target standard deviation (22% in the case of this proficiency test), 79% of the laboratories achieved z scores of less than ¦2¦. The results were evaluated further on the basis of the returned questionnaire that each participant received. The questions asked were focussed on the fact that future method development, if necessary, could be supported by comparison of the methodologies and method procedures applied.JRC.D.8-Food safety and qualit

Validation of an Analytical Method to Determine the Content of Sucralose in Beverages - Report on a Method Validation by Collaborative Study Determination of Sucralose in Beverages by Thin Layer Chromatography in Combination with Reagent-free Derivatisation and Ultraviolet/Fluorescence Detection

An inter-laboratory comparison was carried out to evaluate the performance characteristics of a method for the determination of sucralose in beverages, which was developed at the JRC-IRMM. The method is based on high-performance thin layer chromatography (HPTLC), and reagent-free derivatisation followed by ultraviolet/fluorescence detection. It was tested for the determination of Sucralose (C12H19Cl3O8; (2R,3R,4R,5S,6R)-2-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxy-oxolan-2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3,4-diol; CAS No: 56038-13-2) in carbonated and still alcoholic and non-alcoholic beverages at proposed European regulatory limits according to Directive 2003/115/EC ( ). Precise determination of Sucralose levels in some of the matrices for which European legislative limits apply, required a robust and reliable analytical method. HPTLC employing reagent-free derivatisation offered such a reliable but simple, fast, cost-effective and environment friendly method (very limited quantities of organic solvents methanol and acetonitrile were used). Separation of Sucralose was performed by direct application of samples (diluted, degassed and/or filtered, if necessary) on amino-bonded silica gel HPTLC plates without prior cleanup and development with acetonitrile:water. The sweetener was determined after heating of the developed plate to 190°C and quantified both in ultraviolet absorption and fluorescence measurement mode. Beverages spiked with sucralose as well as beverages taken from the market and labelled to contain sucralose, were sent to 14 laboratories in five different countries following IUPAC guidelines. A sample that did not contain measureable amounts of sucralose was spiked at levels of 30.5 mg/L, 100.7 mg/L and 299 mg/L. Recoveries ranged from 104 ¿ 125 % with an average of 112 % for ultraviolet detection and from 98 ¿ 101 % with an average of 100 % for fluorescent detection. Based on results for spiked samples (blind duplicates at three levels), as well as samples containing Sucralose (blind duplicates at three levels and one split level), the relative standard deviation for repeatability (RSDr) ranged from 10 ¿ 31 % for ultraviolet detection and from 9 ¿ 16 % for fluorescence detection. The relative standard deviation for reproducibility (RSDR) ranged from 14 ¿ 31 % for ultraviolet detection and from 9 ¿ 21 % for fluorescence detection. The limit of quantification on the basis of 10x the baseline noise was 6 mg/L and response was linear in the range between 30 ¿ 150 ng/spot. The method is therefore considered suitable for the determination of Sucralose in beverages at the proposed European legislative limits.JRC.D.8-Food safety and qualit