Background: Monochloropropanediol (MCPD) and its fatty acid esters as well as glycidyl fatty acid esters are substances generated during oil refining or food processing. The free form released during digestion, 3-MCPD and glycidol, have shown adverse effects in animal studies. Objective: So far, the available analytical methods have not been validated in a collaborative study for infant and adult nutritional formulas. This manuscript describes a single-laboratory validation method in view of a future multilaboratory validation trial. Methods: The method described is for the direct determination of 2- and 3-MCPD and indirect determination of 2- and 3-MCPD esters and glycidyl esters in infant and adult/pediatric nutritional formulas by GC coupled to MS. Results: The analytical range was found to be 4–2000 μg/kg powder formula and 0.7–333 μg/kg liquid formula for fatty acid esters of MCPD and glycidol, and 2.5–750 μg/kg samples for free MCPD. The recovery rates were within 91–124% for all samples. Repeatability precision was <20% at levels close to the LOQ. Conclusions: The results met the Standard Method Performance Requirements® (SMPR) set by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals. Highlights: The AOAC Expert Review Panel approved the present method as AOAC Official First Action 2018.03.
Background: In September 2015, both AOAC Official Methods 2015.07and 2015.08 single-laboratory validations (SLVs) were reviewed against Standard Method Performance Requirements® (SMPR) 2014.015by the AOAC Stakeholder Panel for Infant Formula andAdult Nutritional (SPIFAN) Expert Review Panel (ERP). Looking at the similarity and uniqueness of the two methods, the authors agreed, as advised by the ERP, to work together to merge the two methods intoone. This combined method was assigned Method 2016.03. Objective: In order to determine the repeatability and reproducibility of the AOAC First Action 2016.03 method, a collaborative study was organized. The study was divided in two parts: (Part 1) method set up and qualification of participants and (Part 2) collaborative study participation. During Part 1, each laboratory was asked to analyze two practice samples. The laboratories that provided results within a range of expected levels were qualified for Part 2, during which they analyzed 25 samples in blind duplicates. Results: The results were compared with SMPR 2014.015 established for chloride. The precision results (repeatability and reproducibility) were within therequirements stated in the SMPR. In general, the precision results (repeatability and reproducibility)were well within the limits stated in the SMPR. Repeatability ranged from 0.4 to 1.9%, in accordance with data obtained during SLV, with reported RSD of repeatability from 0.03 to 1.6%. Meanwhile, reproducibility ranged from 0.6 to 4.0%. Finally, the Horwitz ratio values were all below 1, from 0.2 to 0.9%. Conclusions: The ERP determined that the data presented met the SMPR and accordingly recommended the method to be granted Final Actionstatus. In January 2018, the Official Methods Boardapproved the method as Final Action.
Background: An acid hydrolysis ultrahigh-performance LC–UV method was evaluated for the determination of total amino acids in infant formula and adult/pediatric nutritional formula. Objective: It was assessed for compliance against AOAC INTERNATIONAL Standard Method Performance Requirements (SMPR®) established by the Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN). Methods: A single-laboratory validation (SLV) study was conducted as a first step in the process to validate the method. In this SLV, 17 SPIFAN matrices representing a range of infant formula and adult nutritional products were evaluated for their amino acid content. Results: The analytical range was found to be within the needs for all products; some may require a dilution. Evaluation of trueness performed on Standard Reference Material 1849a (Infant/Adult Nutritional Formula) showed all compounds met the SMPR theoretical value, with exceptions for threonine and tyrosine. These may have a bias for the National Institute of Standards and Technology (NIST) data, depending on hydrolysis used in the determination of the NIST certificate of analysis. Conclusions: Based on the results of this SLV, this method met the SMPR and was approved as a First Action method by the AOAC Expert Review Panel on Nutrient Methods on August 28, 2018.
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