AOAC 133rd Annual Meeting - Final Program

2:00 PM The Importance of Methods Selection and Validation for Ensuring the Safety and Quality of Botanical Dietary Supplements Paula N. Brown, British Columbia Institute of Technology Product quality and authenticity has been a concern at the fore- front of the natural products industry for decades. Unfortunately, many botanical products in the market today differ substantially in form, potency and even route of administration from traditional herbal medicines. With a multitude of ingredient combinations seen in products that not only incorporate previously unseen herbals, but the addition of technical ingredients such as flavorings and emulsifiers, it is difficult to justify the relationship between history of safe use and modern safety for these prod- ucts. The measurands selected to represent quality determinants, in particular for identity, must too evolve to ensure they are fit for their intended purpose. Univariate measurements of phyto- chemicals in an analytical method validation framework already exist; however, combining such quantitative measurements with an identity parameter is highly desirable but challenging to do. Very limited literature exists in providing guidance in the authentication of botanical-based products in a practical sense. The challenges presented by a continuously changing botanical product landscape will be discussed along recent approaches employed to interpret plant secondary metabolite data sets for authentication and improved safety. 2:30 PM Assessing Vitamin D Status – Analytical Challenges and Accomplishments Stephen A. Wise, Adam J. Kuszak, National Institutes of Health, Johanna Camara, Carolyn Q. Burdette, Grace Hahm, U.S. National Institute of Standards and Technology, Christopher T. Sempos, Vitamin D Standardization Program LLC In 2010, the Office of Dietary Supplements at the National Institutes of Health (NIH-ODS) initiated an international effort to assist in the standardization of measurements for the determi- nation of a clinically-significant nutritional marker for vitamin D status, i.e., 25-hydroxyvitamin D [25(OH)D], which is defined as the sum of 25-hydroxyvitamin D 2 and 25-hydroxyvitamin D 3 . Established as the Vitamin D Standardization Program (VDSP), this effort involves collaboration among NIH-ODS, the National Institute of Standards and Technology (NIST), and vitamin D researchers worldwide. Outputs of the VDSP include the devel- opment of higher-order reference measurement procedures (RMPs) based on liquid chromatography-tandem mass spec- trometry (LC-MS/MS), the development of Standard Reference Materials ® (SRMs) to provide quality assurance of 25(OH)D measurements, interlaboratory assessments of the commutability

of SRMs and external quality assessment samples, and inter- laboratory assessments of the performance of routinely used immunoassay-based tests and LC-MS/MS methods. In this presentation, the analytical challenges associated with accurate assessment of vitamin D status will be discussed, and selected accomplishments of the VDSP to improve the comparability of measurements of 25(OH)D will be highlighted, including the development of SRMs and results of recent interlaboratory comparisons assessing assay performance. SYMPOSIUM: Recent Trends in Elemental Analysis Applications 1:30 PM – 3:00 PM Grand Ballroom 2 Chairs: Kevin Kubachka, U.S. Food and Drug Administration 1:30 PM Arsenic Speciation in Krill Oil by Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry Katarzyna Banaszewski, Anna Plocicka-Okladlo, Aaron Secrist, NOW Foods In recent years, the global demand for krill oil has been on the rise. The increasing popularity of this dietary ingredient has led to increased scrutiny by standard setting bodies and government regulations around the world. In December of 2017, the Food Chemicals Codex (FCC), released a monographed standard for krill oil. The aim of the monograph was to help promote quality krill oil identification and purity testing to strengthen the position of krill in the marketplace. Included in the requirements for krill oil are standards for EPA, DHA, phospholipids and astaxanthin. The monograph also included a limit for inorganic arsenic at NMT 0.1 mg/kg. The method defined in the monograph, which is not able to accurately differentiate between the chemical species of arsenic, cannot be compared with higher sensitivity and specific- ity speciation methods, such as HPLC-ICP-MS. Additionally, the complexity of the krill oil matrix requires suitable sample prepa- ration able to liberate arsenic species and allow for precise quantitation of inorganic arsenic. To address the lack of an official method, a study was conducted to develop and validate a procedure for arsenic speciation in krill oil samples and thus contribute to a more accurate risk assessment analysis.

WWW.AOAC.ORG 301.924.7077 7