Melissa M Phillips1, Tomás M López Seal1, Jennifer M Ness2, Kai Zhang3. 1. U.S. National Institute of Standards and Technology (NIST), Chemical Sciences Division, Gaithersburg, MD. 2. U.S. National Institute of Standards and Technology (NIST), Chemical Sciences Division, Charleston, SC. 3. U.S. Food and Drug Administration (FDA), Center for Food Safety and Applied Nutrition, Office of Regulatory Science, College Park, MD.
Abstract
Background: Matrix-matched reference materials (RMs) are critical for adequate quality assurance of extraction, digestion, separation, and/or detection processes for analytes of interest in foods and dietary supplements. The accurate determination of mycotoxins in foods is an international concern. While RMs for mycotoxins are available from a variety of RM producers, these mainly address a single mycotoxin or group of mycotoxins and therefore require the use of multiple RMs for multitarget methods. Objective: To address the increasing needs of laboratories moving toward LC-MS-based multimycotoxin analysis, the U.S. National Institute of Standards and Technology (NIST) collaborated with the U.S. Food and Drug Administration (FDA) to produce a naturally incurred RM for multiple mycotoxins in corn. Methods: Homogeneity of the RM has been assessed using a stratified random sampling of the final product based on mycotoxin mass fractions measured by the FDA and NIST. Multiple sample sizes were evaluated to maximize homogeneity in the obtained results. The mycotoxin levels in the final materials have been evaluated via interlaboratory comparison and isotope dilution LC-tandem MS measurements made at the FDA and NIST. The final value assignment combined results from these data sets. Conclusions: The study successfully developed a certified RM, SRM 1565 Mycotoxins in Corn, and a workflow for the future development of multimycotoxin RMs in different matrices.
Background: Matrix-matched reference materials (RMs) are critical for adequate quality assurance of extraction, digestion, separation, and/or detection processes for analytes of interest in foods and dietary supplements. The accurate determination of mycotoxins in foods is an international concern. While RMs for mycotoxins are available from a variety of RM producers, these mainly address a single mycotoxin or group of mycotoxins and therefore require the use of multiple RMs for multitarget methods. Objective: To address the increasing needs of laboratories moving toward LC-MS-based multimycotoxin analysis, the U.S. National Institute of Standards and Technology (NIST) collaborated with the U.S. Food and Drug Administration (FDA) to produce a naturally incurred RM for multiple mycotoxins in corn. Methods: Homogeneity of the RM has been assessed using a stratified random sampling of the final product based on mycotoxin mass fractions measured by the FDA and NIST. Multiple sample sizes were evaluated to maximize homogeneity in the obtained results. The mycotoxin levels in the final materials have been evaluated via interlaboratory comparison and isotope dilution LC-tandem MS measurements made at the FDA and NIST. The final value assignment combined results from these data sets. Conclusions: The study successfully developed a certified RM, SRM 1565 Mycotoxins in Corn, and a workflow for the future development of multimycotoxin RMs in different matrices.