AOAC SMPR 2016.014.

Barcoding animal species

AOAC SMPR 2016.013.

A single-laboratory validation of a method using Folin & Ciocalteu's phenol reagent (Folin-C reagent) for determination of total phenolic content of selected dietary supplement extracts was performed. The method is composed of a water extraction of dried extracts with sonication followed by reaction with the Folin-C reagent. The resulting colorimetric reaction is measured at 765 nm and compared with a standard curve generated with gallic acid standard solutions. The validation results were compared with Standard Method Performance Requirement (SMPR®) 2015.009, developed by the Stakeholder Panel on Dietary Supplements. The method demonstrated acceptable within-day RSDr of 1.96-7.47% for the five matrixes studied (grape seed extract, grape skin extract, black tea extract, green coffee extract, and cocoa extract). When gallic acid was spiked into maltodextrin (a surrogate dietary supplement carrier) at 30 or 70%, the recovery ranged from 91 to 104%, within the acceptable range established by SMPR 2015.009. Selectivity testing with glucose, fructose, and sucrose demonstrated no positive interference by these compounds. Finally, ruggedness studies demonstrated no significant effects due to changes in the heating apparatus, test material weight, read time after reaction, amount of Folin-C reagent, reaction time, reaction temperature, and amount of Na2CO3. The single-laboratory validation results support adoption of the method as First Action Official MethodSM 2017.13 and further evaluation in a collaborative study.

AOAC SMPR® 2017.009. Standard Method Performance Requirements (SMPRs) for Quantitation of Aloe Vera Characteristic Water-Soluble Main Constituents in Dietary Supplements.

Standard Method Performance Requirements (SMPRs®) 2018.004: Determination of trans Resveratrol in Dietary Supplements and Dietary Ingredients.

What: AOAC Standard Method Performance Requirements (SMPRs) are voluntary consensus standards developed in accordance with the AOAC policy, "AOAC Due Process for Development of AOAC Non-Method Consensus Standards and Documents." SMPRs describe a scientific community's recommended minimum method performance characteristics and analytical requirements for a specific method related intended use.

AOAC Standard Method Performance Requirements (SMPRs ) describe the minimum recommended performance characteristics to be used during the evaluation of a method. The evaluation may be an on-site veri cation, a single-laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by AOAC stakeholder panels composed of representatives from industry, regulatory organizations, contract laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC expert review panels (ERPs) in their evaluation of validation study data for methods being considered for

AOAC SMPR® 2011.006.

AOAC Standard Method Performance Requirements (SMPRs ) describe the minimum recommended performance characteristics to be used during the evaluation of a method. The evaluation may be an on-site veri cation, a single-laboratory validation, or a multi-site collaborative study. SMPRs are written and adopted by AOAC stakeholder panels composed of representatives from industry, regulatory organizations, contract laboratories, test kit manufacturers, and academic institutions. AOAC SMPRs are used by AOAC expert review panels in their evaluation of validation study data for method being considered for Performance Tested Methods or AOAC O cial Methods of Analysis , and can be used as acceptance criteria for veri cation at user laboratories.

Standard Method Performance Requirements (SMPRs®) 2017.021: Quantitation of Wheat, Rye, and Barley Gluten in Oats.

Standard Method Performance Requirements (SMPRs®) 2017.020: Quantitation of Chicken Egg by ELISA-Based Methods.

A multi-laboratory study was completed for AOAC First Action Method 2015.14. Ten laboratories from eight countries participated. Each laboratory analyzed (in duplicate) a placebo and 14 fortified nutritionals. Product matrices analyzed included milk, soy, partially hydrolyzed milk, partially hydrolyzed soy, and elemental-based infant formula powders, milk based infant formula ready-to-feed liquids, adult low-fat powders, and adult high fat and high protein ready-to-drink nutritionals. Data was then compared to standard method performance requirements (SMPR). Samples were prepared by enzymatic digestion with papain, α-amylase, and phosphatase to hydrolyze protein and complex carbohydrate and to free phosphorylated vitamin forms respectively. Stable-isotope labeled internal standards were incorporated into the sample preparation to correct for variability in both the sample preparation and instrument response. Prepared samples and working standard solutions were injected onto an ultra-high-pressure liquid chromatograph, interfaced to a triple-quadrupole mass spectrometer (MS/MS). Reverse phase gradient chromatography, using mobile phases of methanol and 20 mM ammonium formate in water on a C-18 column, were used for the analysis. The MS/MS was configured to monitor precursor-fragment ion pairs for each analyte and internal standard. Vitamins B1 (thiamine), B2 (riboflavin), B3 (niacin), and B6 (pyridoxine) were quantified by least squares regression using the response ratio of the analyte to its internal standard. Total vitamins B1, B2, B3, and B6 had average repeatability of 2.3%, 3.9%, 2.7%, and 2.2% RSD, and reproducibility of 8.2%, 6.9%, 6.7%, and 5.8% RSD, respectively. Repeatability and reproducibility SMPR were met for 53/56 and 50/56 fortified-product/analyte pairs analyzed, respectively.

Chlorate is an effective herbicide, but also a by-product of chlorinating agents used to disinfect water, one of the reasons why it is regularly found in food. Perchlorate is a ubiquitous contaminant, which is naturally occurring in the environment but also released from anthropogenic sources such as the industrial use of certain natural fertilizers. Chlorate affects the hematological system, and perchlorate the thyroid. Implement and validate a simple and robust analytical method for the accurate determination of chlorate and perchlorate in baby food, infant and adult formulas, and ingredients thereof, which is suited for its application in routine environments where a broad variety of food commodities must be analyzed simultaneously. Typically, analytes are extracted with a mixture of water, acidified methanol and dichloromethane. Optionally, for dairy products and byproducts, extraction can be performed with water, acidified methanol and EDTA, followed by two steps clean-up (freezing-out and dispersive solid phase extraction with C18 in acetonitrile). Quantitative determination is carried out by isotopic dilution liquid chromatography tandem mass spectrometry (LC-MS/MS). The method was single laboratory validated in five Nestlé Quality Assurance Centers (NQACs) in a comprehensive range of representative matrices of different categories such as baby foods, infant/adult formulas and ingredients, with results generally in agreement with the acceptance criteria of the Standard Method Performance Requirements (SMPR) 2021.001 defined by AOAC INTERNATIONAL, in terms of representative matrices validated, LOQs, trueness and precision.

A GC/MS method focusing on the characterization and quantification of ginkgolic acids (GAs) in Ginkgo biloba L. plants, extracts and dietary supplements was developed. The analysis was performed on a HP-88 column. The GAs were derivatized with trimethylsulfonium hydroxide [(CH3)3SOH]. By using this technique, separation of 2 saturated (C13:0 and C15:0) and 6 unsaturated ginkgolic acid methyl esters with different positional double bonds (C15:1 Δ8 and Δ10, C17:1 Δ8, Δ10 and Δ12, and C17:2) was achieved. The developed GC/MS method was validated and the quantitation results were verified by comparison with a standard HPLC method. Nineteen G. biloba authenticated and commercial plant samples and 21 dietary supplements purported to contain G. biloba leaf extracts were analyzed. The presence of the marker compounds, terpene trilactones and flavonol glycosides, for Ginkgo biloba in the dietary supplements was determined by UHPLC/MS and used to confirm the presence of G. biloba leaf extracts in all of the botanical dietary supplements.

There is currently no cure for food allergies, and sufferers can only rely on the correct labeling of foods to avoid allergens. Hence, it is important that analytical methods are sensitive and accurate enough to screen for the presence of multiple allergens in food products. In this study, we developed an LC-tandem MS method that is able to simultaneously screen or quantify the signature tryptic peptides of multiple allergen commodities. This method is capable of screening and identifying egg white, skim milk, peanut, soy, and tree nuts (almond, Brazil nut, cashew, hazelnut, pecan, pine nut, pistachio, and walnut) at a detection limit of 10 ppm in incurred bread and cookies. It was further tested for the quantitative analysis of whole-egg, whole-milk, peanut butter, and hazelnut commodities, which are incurred or spiked into selected food matrixes as defined in AOAC INTERNATIONAL Standard Method Performance Requirement (SMPR®) 2016.002. The method demonstrated excellent sensitivity with a Method quantitative limit of 3 ppm for whole egg and 10 ppm for the remaining three allergen commodities. It also demonstrated good recovery (60-119%) and repeatability (RSDr <20%), with an analytical range of 10-1000 ppm for each allergen commodity and was able to meet the minimum performance requirements of the SMPR.