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Confidential Business Information
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Ethanol Industry Mycotoxin Task Group
Industry Task Group Formed > 5 B gallons represented from producers 8 Commercial Labs University and Government Representatives First Task Group Meeting: Friday, April 7, 2017 Task Group has met 10 times in 6 months Started a best practices white paper task group at AAFCO Performed 3 Inter-Laboratory Studies (ILS) Focus has been on DON initially; other toxins are of interest to the group as well 3P Lab Group CV = 38%
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Additional Background
Started out as an effort to standardize the test methods for mycotoxin analysis of DDGS – similar in concept to the effort we undertook in 2007 regarding proximate analysis of DDGS: Evaluation of Analytical Methods for Analysis of Dried Distillers Grains with Solubles -AFIA Sub-Working Group Final Report and Recommendations, February 2007 Quickly modified the scope to focus on getting the results between labs to agree regardless of the method utilized Confidential Business Information
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Evaluation of Analytical Methods for Analysis of Dried Distillers Grains with Solubles
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Inter-Laboratory Studies
Samples of naturally contaminated DDGS are split with a riffle splitter and sent to participating labs Also prepared a Known Value Reference Material – prepared by the gravimetric addition of pure toxin in a known non-detectable substrate Labs analyze samples in triplicate, allowing for both precision and accuracy to be evaluated Precision is measured by the Intra and Inter-Laboratory Coefficient of Variation of the triplicates Accuracy is measured by: 1) the z-score of each lab – i.e. degree of variance from the Group Mean and 2) the % recovery of a known value reference material
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Individual Lab Performance
Following charts are for each participating lab individually CV chart is on the left; z-score chart is on the right All charts are scaled identically to display performance relative to the group 1 sample excluded from ILS #1 because it was a ND for DON – all labs performed similarly on this sample Lab-734 does not have a calculated CV for ILS #3 because they have only reported 1 result for each sample as of (10/9/17)
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Lab-109
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Lab-158
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Lab-217
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Lab-263
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Lab-498 Confidential Business Information
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Lab-506
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Lab-734
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Lab-787
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ILS #1 8 Participating Labs 3 Samples
1 of the samples was excluded from this analysis/presentation because it was a ND – all labs performed similarly on this excluded sample Samples were split and shipped to labs Labs analyzed each sample in triplicate and reported the results
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ILS #1 – DON-5
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ILS #1 – DON-9
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ILS #2 8 Participating Labs 5 Samples
DON-12 sample was a known value DDGS sample – prepared by gravimetric addition of pure DON Toxin = ppm Samples were split and shipped to labs Labs analyzed each sample in triplicate and reported the results
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ILS #2 – DON-1
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ILS #2 – DON-2
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ILS #2 – DON-12 (13.65ppm)
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ILS #2 – DON-16
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ILS #2 – DON-20
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ILS #3 8 Participating Labs 3 Samples DON-6 sample was a known value DDGS sample – prepared by gravimetric addition of pure DON Toxin = ppm Samples were split and shipped to labs Labs analyzed each sample in triplicate and reported the results
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ILS #3 – DON-6 (10.87ppm)
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ILS #3 – DON-7
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ILS #3 – DON-15
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Conclusions Tremendous improvement has been made on both inter-laboratory variability and % recoveries Variation reduction is approaching a diminishing return, signaling we may have obtained most of the benefit achievable Lab 734 is the hold out and still needs to significantly improve their % recovery of DON – if Lab 734 falls in line, variation will be at a manageable level Move efforts to other toxins (Aflatoxin, Fumonison, and Zearalenone)
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