Darryl Sullivan

Determination of Total Iodine in Infant Formula and Adult/ Pediatric Nutritional Formula by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS): Collaborative Study, Final Action 2012.15.

A collaborative study was conducted to determine total iodine in infant formula and adult/pediatric nutritional formula by inductively coupled plasma-MS (ICP-MS) using AOAC First Action Official Method(SM) 2012.15. The purpose of this study was to evaluate the methods intralaboratory and interlaboratory performance and submit the results to AOAC INTERNATIONAL for adoption as a Final Action Official Method for the determination of total iodine in infant formula and adult/pediatric nutritional formula. Upon providing acceptable results for practice samples National Institute of Standard and Technology (NIST) Standard Reference Material (SRM) 1849a and a low-fat adult nutritional powder, 13 laboratories analyzed seven various infant and adult nutritional products including a blind duplicate of each. Products were chosen with varying levels of iodine and included low-fat, soy-based, and milk-based formulas and NIST SRM 1849a. Random identification numbers were assigned to each of the seven fortified test materials. Digestion of the test samples occurred using a potassium hydroxide solution in an oven or open-vessel microwave system. Iodine was stabilized with ammonium hydroxide and sodium thiosulfate after digestion. The solutions were brought to volume followed by filtration. The filtrates were then analyzed by ICP-MS after dilution. Results for all seven test samples met all the AOAC Standard Method Performance Requirements (SMPR(®) 2012.008) guidelines. The RSDr ranged from 0.77 to 4.78% and the RSDR from 5.42 to 11.5%. The Horwitz ratio (HorRat) for each result was excellent, ranging from 0.35 to 1.31%. The results demonstrate that the method is fit-for-purpose to determine iodine in infant formula and adult/pediatric nutritional formula.

Modernization of AOAC Nutrient Methods by Stakeholder Panel on Infant Formula and Adult Nutritionals.

Infant formula is one of the most highly regulated products in the world. To comply with global regulations and to ensure the products are manufactured within product specifications, accurate analytical testing is required. Most of the AOAC INTERNATIONAL legacy test methods for infant formula were developed and validated in the 1980s and 1990s. Although these methods performed very well for many years, infant formulas have been updated, and todays products contain many new and novel ingredients. There were a number of cases in which the legacy AOAC methods began to result in problems with the analysis of modern infant formulas, and the use of these methods caused some disputes with regulatory agencies. In 2010, AOAC reached an agreement with the International Formula Council, which has changed its name to the Infant Nutrition Council of America, regarding a project to modernize these AOAC infant-formula test methods. This agreement led to the development of Standard Method Performance Requirements (SMPRs(®)) for 28 nutrients. After SMPR approval, methods were collected, evaluated, validated, and approved through the AOAC Official Methods(SM) process. Forty-seven methods have been approved as AOAC First Action Methods, and eight have been approved as Final Action.

Evaluation Protocol for Review of Method Validation Data by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals Expert Review Panel.

Methods under consideration as part of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals process are to be evaluated against a set of Standard Method Performance RequirementsSM (SMPRs) via peer review by an expert review panel (ERP). A validation protocol and a checklist have been developed to assist the ERP to evaluate experimental data and to compare multiple candidate methods for each nutrient. Method performance against validation parameters mandated in the SMPRs as well as additional criteria are to be scored, with the method selected by the ERP proceeding to multilaboratory study prior to Final Action approval. These methods are intended to be used by the infant formula industry for the purposes of dispute resolution.

Development and Validation of Analytical Methods to Ensure the Quality and Safety of Dietary Supplements

Publisher Summary The expanding use of innovative botanical ingredients in dietary supplements and foods has resulted in a flurry of research aimed at the development and validation of analytical methods for accurate measurement of active ingredients. The analysis of food and dietary supplements is constantly evolving in order to keep pace with new, innovative ingredients and products. The explosion in the use of botanical ingredients and nutraceutical products is perhaps one of the most challenging tasks to face the analytical community. The tremendous popularity of these products has resulted in increased scrutiny from consumers, health professionals and regulators about the quality and levels of active ingredients in these products. The ultimate goal is to address and overcome the challenges associated with the analysis of the products. Many of these hurdles are not encountered by other types of products in developing and validating analytical methods for dietary products. The active constituents are not known and appropriate marker substances must be selected. The natural variability of many of these products also complicates method development and validation. When instability of many of the active components and marker compounds after removal from the plant matrix is factored in, the need for agreement on a single, rugged, thoroughly validated analytical method becomes clear.