TRILOGY REFERENCE MATERIAL CERTIFICATE OF ANALYSIS

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1 TRILOGY REFERENCE MATERIAL CERTIFICATE OF ANALYSIS Certification Date: August, 2017 Expiration date: August, 2022 Product Name: Multitoxin Reference Material Product Number(s): TR-MT100, TR-MT500, TR-MT1000 Batch number: MT-C-9999J Product Size(s): 100 grams, 500 grams, or 1000 grams Product description: Corn naturally contaminated with mycotoxins. This finely ground product is packaged in appropriately sized zippered sealed foil pouches. AFLATOXIN Certified Values Aflatoxin B1 1.0 ppb 12.3 (ug/kg) Aflatoxin B2 1.0 ppb 0.7 (ug/kg) Aflatoxin G1 1.0 ppb 0.7 (ug/kg) Aflatoxin G2 1.0 ppb ND (ug/kg) Total Aflatoxins 13.7 ppb (ug/kg) 2.7 ppb (ug/kg) %CV or %RSD 19.5 % Aflatoxin Standard Deviation and Measurement Uncertainty Ranges 1 sd range = 11.0 ppb to 16.4 ppb 2 sd range = 8.3 ppb to 19.1 ppb 3 sd range = 5.6 ppb to 21.8 ppb Aflatoxin Expanded Measurement of Uncertainty k = 2: 5.5 ppb or 40.5 % Range of Product incorporating uncertainty range: 8.1 ppb to 19.2 ppb Aflatoxin Method Reference AOAC with modifications. Includes KOBRA Cell Derivitazition 1

2 FUMONISIN - Certified Values Compound Quantification ppm SI Units Fumonisin B1 0.1 ppm 6.0 (mg/kg) Fumonisin B2 0.1 ppm 1.9 (mg/kg) Fumonisin B3 0.1 ppm 0.6 (mg/kg) Total Fumonisins 8.5 ppm (mg/kg) 0.5 ppm (mg/kg) %CV or %RSD 5.5 % Fumonisin Standard Deviation and Measurement Uncertainty Ranges 1 sd range = 8.0 ppm to 9.0 ppm 2 sd range = 7.5 ppm to 9.5 ppm 3 sd range = 7.0 ppm to 10.0 ppm Fumonisin Expanded Measurement of Uncertainty k = 2: 1.6 ppm or 18.3 % Range of Product incorporating uncertainty range: 7.0 ppm to 10.1 ppm Fumonisin Method Reference AOAC # with modifications. Fluoresence detection and NDA derivitatization. OCHRATOXIN A - Certified Values Ochratoxin A 1.0 ppb 8.6 (ug/kg) Total Ochratoxin A 8.6 ppb (ug/kg) 1.8 ppb (ug/kg) %CV or %RSD 20.8 % Ochratoxin Standard Deviation and Measurement Uncertainty Ranges 1 sd range = 6.8 ppb to 10.4 ppb 2 sd range = 5.0 ppb to 12.2 ppb 3 sd range = 3.2 ppb to 14.0 ppb Ochratoxin Expanded Measurement of Uncertainty k = 2: 3.7 ppb or 43.5 % Range of Product incorporating uncertainty range: 4.8 ppb to 12.3 ppb Ochratoxin Method Reference LC-MS/MS Internal SOP Matrix Matched Standards. QTrap 5500 LC-MS/MS System. 2

3 Zearalenone - Certified Values Zearalenone 50 ppb (ug/kg) Total Zearalenone ppb (ug/kg) 61.6 ppb (ug/kg) %CV or %RSD 18.6 % Zearalenone Standard Deviation and Measurement Uncertainty Ranges 1 sd range = ppb to ppb 2 sd range = ppb to ppb 3 sd range = ppb to ppb Zearalenone Expanded Measurement of Uncertainty k = 2: ppb or 41.5% Range of Product incorporating uncertainty range: ppb to ppb Zearalenone Method Reference LC-MS/MS Internal SOP Matrix Matched Standards. QTrap 5500 LC-MS/MS System. DEOXYNIVALENOL (DON) Certified Values Compound Quantification ppm SI Units Deoxynivalenol (DON) 0.1 ppm 2.7 (mg/kg) Total Deoxynivalenol 2.7 ppm (mg/kg) 0.1 ppm (mg/kg) %CV or %RSD 4.8 % Deoxynivalenol Standard Deviation and Measurement Uncertainty Ranges 1 sd range = 2.6 ppm to 2.8 ppm 2 sd range = 2.5 ppm to 2.9 ppm 3 sd range = 2.4 ppm to 3.0 ppm Deoxynivalenol Expanded Measurement of Uncertainty k = 2: 0.4 ppm or 13.9 % Range of Product incorporating uncertainty range: 2.3 ppm to 3.0 ppm Deoxynivalenol Method Reference Truckess, Et. Al. Journal of AOAC Vol. 81, No 4, With Modifications 3

4 T-2 TOXIN - Certified Values T-2 Toxin 5 ppb (ug/kg) Total T-2 Toxin ppb (ug/kg) 40.2 ppb (ug/kg) %CV or %RSD 12.1 % T-2 Toxin Standard Deviation and Measurement Uncertainty Ranges 1 sd range= ppb to ppb 2 sd range = ppb to ppb 3 sd range = ppb to ppb T-2 Expanded Measurement of Uncertainty k = 2: 86.1 ppb or 25.9 % Range of product incorporating uncertainty range: ppb to ppb HT-2 TOXIN - Certified Values HT-2 Toxin 5 ppb (ug/kg) Total HT-2 Toxin ppb (ug/kg) 16.9 ppb (ug/kg) %CV or %RSD 7.1 % HT-2 Toxin Standard Deviation and Measurement Uncertainty Ranges 1 sd range= ppb to ppb 2 sd range = ppb to ppb 3 sd range = ppb to ppb HT-2 Expanded Measurement of Uncertainty k = 2: 40.4 ppb or 16.8 % Range of product incorporating uncertainty range: ppb to ppb T-2/HT-2 Method Reference LC-MS/MS Internal SOP Matrix Matched Standards. QTrap 5500 LC-MS/MS System. General Information This material represents a food/feed agricultural product commonly contaminated with mycotoxins. It has been ground to a fine consistency (30 mesh; mm) and thoroughly homogenized to insure uniform distribution of the analyte(s). Samples are analyzed numerous times over the course of several analytical runs utilizing the reference method listed above. The results are averaged and standard deviation ranges as well as measurement of uncertainty are calculated. All of these are represented above. This data represents the best estimate of the true value as obtained in one laboratory utilizing one method. 4

5 Method Used for Certification: To obtain the results above, 30 different extracts were prepared on a minimum of 6 different analyses dates. For Aflatoxin, DON, Zearalenone, T-2 Toxin and HT-2 Toxin the samples were extracted with 84/16 acetonitrile/water for 1 hour on an eberbach shaker. For Fumonisin and Ochratoxin A the samples were extracted with 3/1 methanol/water and extracted for 1 hour on an eberbach shaker. All samples were analyzed by the method references above. This result represents the results you would find from one laboratory performing one specific method repeatedly over the course of several weeks. The standard deviation ranges notes above represent results you would anticipate with 68% (1 sd range), 95% (2 sd range) and 99% (3 sd range) confidence with the method specifics listed above. Additionally, uncertainty has been calculated and the range is also reported above. These ranges will allow you, the end user to determine which range best suits your individual requirements. Results of this sample may vary with methodology and extraction procedures utilized in your laboratory. These results relate only to the sample material listed above. The certified value is the best estimate of the true value based on these multiple analyses. Minimum Sample Size Results shown above represent 5.0 gram extractions. Increasing the sample size extracted may provide results with tighter ranges. Less than 5 gram sample extractions are not recommended. Intended Use This material is intended for laboratory use only. Some of the intended uses include but are not limited to: Quality control sample, training tools, method comparisons, Method validations, intra laboratory comparisons, and inter laboratory comparisons. This product is for laboratory use only and is not intended for animal or human consumption. Storage Material should be stored below 8 C in the original foil zippered pouch. After opening, insure bag is completely sealed prior to returning to storage. Trilogy Analytical Is not responsible for changes in the product during improper storage of material at a customer s premises. Instructions for Use Allow material to come to room temperature before using to prevent moisture condensation in packet. Recommended minimum subsample is 5 grams. Samples should be sealed promptly and returned to storage conditions after use. The expiration date of this material represents the best current knowledge and is applied to product that has been stored and handled correctly. 5

6 Hazardous situations/health and Safety Observe all standard laboratory safety procedures when handling this material. Use appropriate personal protective equipment including gloves, safety glasses and protective clothing. Level of Homogeneity Mycotoxins are known to exhibit extreme inhomogeneity. These samples have been ground to a fine particle size (30 mesh; mm), to provide the best sample homogeneity available. A minimum sub-sample of 5 grams must be extracted to insure a sample representative of the larger sample received. If smaller samples are taken, results may fall out of range due to sample variability. Likewise, extraction of larger sample sizes may improve the variability of results. Uncertainty The uncertainty of the sample is stated above. Uncertainty is calculated according to the procedures in the Guide to Expression of Uncertainty in Measurement (1). All calculations of expanded uncertainty (k = 2) are based on the criteria outlined in the ISO guide to the expression of uncertainty in measurement (GUM). Expanded combined uncertainty, which is calculated and presented for all Reference Material, represents an estimated standard deviation equal to the root sum squared of all total inherent variance of pertinent components expanded by a factor of 2 (k = 2). The expanding factor k allocates a coverage at which a 95% confidence level (k = 2) can be obtained. Within the Certificate of Analysis for each reference material an expanded range for the product in accordance with the uncertainty is included. For additional information pertaining to individual uncertainty components affecting final result of Trilogy Certified Reference Material please contact. Approved for Release and Distribution by Date: August 14, 2017 Julie Brunkhorst Vice President of the Technical Division References (1) JCGM 100:2008, Evaluation of measurement data, Guide to expression of uncertainty in measurement (2) ISO/IEC Guide 98-1:2009 Uncertainty of measurement, Part 1: Introduction to the expression of uncertainty in measurement. (3) ISO guide 31, (2015). Reference Materials Contents of Certificates and Labels (4) ISO Guide 35, (2006) General and statistical Principles (5) ISO Guide 34, (2009) General requirements for the competence of reference material producer Legal Notices: Trilogy does not make any warranties, express or implied in connection with this product. Trilogy does not guarantee the use of this product for specific applications. Each purchaser should determine the best methods and suitability for this product to meet their specific needs. Trilogy does warranty that this product meets the control standards set by. 6