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

2015 ◽  
Vol 98 (1) ◽  
pp. 112-115 ◽  
Author(s):  
Brendon D Gill ◽  
Harvey E Indyk ◽  
Christopher J Blake ◽  
Erik J M Konings ◽  
Wesley A Jacobs ◽  
...  
Keyword(s):  
Dispute Resolution ◽  
Infant Formula ◽  
Standard Method ◽  
Review Panel ◽  
Validation Data ◽  
Method Performance ◽  
Expert Review ◽  
Evaluation Protocol ◽  
Validation Parameters ◽  
Expert Review Panel

Abstract 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 beendeveloped to assist the ERP to evaluate experimentaldata 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.

Determination of Alkaloids in Mitragyna speciosa (Kratom) Raw Materials and Dietary Supplements by HPLC-UV: Single-Laboratory Validation, First Action 2017.14

2018 ◽  
Vol 101 (4) ◽  
pp. 964-965
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown
Keyword(s):  
Standard Method ◽  
Raw Materials ◽  
Review Panel ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Mitragyna Speciosa ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract The AOAC Expert Review Panel (ERP) approved a method for the quantitation of alkaloids in Mitragyna speciosa for consideration as First Action Official MethodSM status. The previously published method summarized a single-laboratory validation of two alkaloids, mitragynine and 7-hydroxymitragynine, in raw materials and finished products. The methods performance was compared with the AOAC Standard Method Performance Requirement 2015.008. With repeatability precision (RSDr) ranging from 0.51 to 0.95% and recoveries from 93.6 to 98.9% in the different product matrices, the ERP adopted the method and provided recommendations for achieving Final Action status.

scholarly journals Determination of Curcuminoids in Turmeric Raw Materials and Dietary Supplements by HPLC: Single-Laboratory Validation, First Action 2016.16

2018 ◽  
Vol 101 (1) ◽  
pp. 203-207 ◽  
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown
Keyword(s):  
Dietary Supplements ◽  
Standard Method ◽  
Raw Materials ◽  
Review Panel ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract The AOAC Expert Review Panel (ERP) approved a method for the quantitation of curcuminoids for consideration for First Action Official MethodSM status. The previously published method summarized a single-laboratory validation of three individual curcuminoinds—curcumin, demethoxycurcumin, and bis-demethoxycurcumin—in raw materials and finished products. Method performance was compared with AOAC Standard Method Performance Requirement 2016.003. With repeatability precision ranging from 0.3 to 5.5% and recoveries from 96.6 to 103.3% in the different product matrixes, the ERP adopted the method and provided recommendations for achieving Final Action status.

Vitamin C in Infant Formula and Adult/Pediatric Nutritional Formula by HPLC with UV Detection: First Action 2012.21

2013 ◽  
Vol 96 (4) ◽  
pp. 802-807 ◽  
Author(s):  
Karen Schimpf ◽  
Linda Thompson ◽  
Steve Baugh
Keyword(s):  
Ascorbic Acid ◽  
Vitamin C ◽  
Infant Formula ◽  
Review Panel ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel

Abstract This method for the determination of vitamin C by HPLC allows for the separation and quantitation of L-ascorbic acid in infant, pediatric, and adult nutritional products. Liquids, semisolids, and powders ranging from 2 to 1000 mg/kg in their consumable forms were analyzed during the method validation. The method met the standard method performance requirements and was approved by an AOAC Expert Review Panel on Infant Formula and Adult Nutritionals on October 2, 2012. During validation, the overall intermediate precision was 2.1% RSD (triplicate determinations on 7–10 days); the within-day precision, or repeatability, was 1.54% RSD (triplicate determinations). Accuracy, as spike recovery, ranged from 97.0 to 100.9%. The method detection and quantitation limits were determined experimentally to be 0.02 and 0.06 mg/L, respectively, in prepared samples.

scholarly journals Chloride in Milk, Milk Powder, Whey Powder, Infant Formula, and Adult Nutritionals Potentiometric Titration: Collaborative Study, Final Action 2016.03

2019 ◽  
Vol 102 (2) ◽  
pp. 564-569
Author(s):  
Greg Jaudzems ◽  
Fengxia Zhang ◽  
Wu Bolong ◽  
Lei Bao ◽  
Jing Xiao
Keyword(s):  
Infant Formula ◽  
Collaborative Study ◽  
Milk Powder ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility ◽  
Set Up ◽  
Single Laboratory

Abstract 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.

Total Iodine in Infant Formula and Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: First Action 2012.14

2013 ◽  
Vol 96 (4) ◽  
pp. 798-801 ◽  
Author(s):  
Lawrence H Pacquette ◽  
Alan M Levenson ◽  
Joseph J Thompson ◽  
Dawn Dowell
Keyword(s):  
Infant Formula ◽  
Inductively Coupled Plasma ◽  
Internal Standard ◽  
Total Iodine ◽  
Method Performance ◽  
Inductively Coupled ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Plasma Mass Spectrometry

Abstract After an assessment of data generated from a single-laboratory validation study published in the Journal of AOAC INTERNATIONAL 95, 169–176 (2012), a method for determining the total level of iodine in infant formula and nutritional products was presented for consideration for adoption by AOAC during the AOAC Annual Meeting held September 30–October 3, 2012 in Las Vegas, NV. An Expert Review Panel on Infant Formula and Adult Nutritionals concluded that the method met the established standard method performance requirements, and approved the method as AOAC Official First Action. The method involves digestion of the sample with nitric acid in a closed vessel microwave oven, followed by determination by inductively coupled plasma/MS using tellurium as the internal standard. The method LOQ for total iodine was 1.5 μg/100 g, but a practical LOQ was used at 5 μg/100 g total iodine. The analytical range of the method was 5–100 μg/100 g total iodine. The recoveries from 15 spiked nutritional products ranged from 90 to 105%.

Determination and Confirmation of Parent and Total Ractopamine in Bovine, Swine, and Turkey Tissues by Liquid Chromatography with Tandem Mass Spectrometry: First Action 2011.23

2012 ◽  
Vol 95 (5) ◽  
pp. 1235-1255 ◽  
Author(s):  
Thomas J Burnett ◽  
John M Rodewald ◽  
Sharon L Brunelle ◽  
Mark Neeley ◽  
Michael Wallace ◽  
...  
Keyword(s):  
Internal Standard ◽  
Veterinary Drug ◽  
Review Panel ◽  
Validation Data ◽  
Expert Review ◽  
Maximum Residue Limits ◽  
Initial Extract ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A candidate method selected by the AOAC Expert Review Panel (ERP) for Ractopamine for determination and confirmation of parent and total ractopamine by LC/MS/MS was validated in a single laboratory for bovine, swine, and turkey tissues. The candidate method utilizes methanol extraction of the tissues, followed by an optional enzymatic hydrolysis for determination of total (parent plus conjugate) ractopamine. A mixed-mode cation exchange SPE cartridge is used to purify the initial extract before LC/MS/MS. Matrix-matched standards and a ractopamine-d6 internal standard are used for quantification of parent and total ractopamine in unknown samples. Validation data demonstrated that mean intertrial recoveries for ractopamine across all concentrations tested ranged from 79.7 to 102.2% for parent ractopamine and from 79.0 to 100.0% when a hydrolysis step was included. Intertrial repeatability precision ranged from 2.44 to 11.1% for parent ractopamine and 4.97 to 15.0% with hydrolysis. Estimated LOD values were below 0.1 ng/g and LOQ values were validated at 0.25x the maximum residue limits. The data satisfy the requirements of the AOAC Stakeholder Panel for Veterinary Drug Residue Methods for single laboratory validation studies. The method was awarded Official Methods of AnalysisSM First Action 2011.23 by the AOAC ERP on Veterinary Drug Residues.

Vitamin C in Infant Formula and Adult/Pediatric Nutritional Formula by Liquid Chromatography with UV Detection: Collaborative Study, Final Action 2012.22

2017 ◽  
Vol 100 (1) ◽  
pp. 139-144 ◽  
Author(s):  
Esther Campos Giménez ◽  
Frédéric Martin ◽  
K Schimpf ◽  
L Butler Thompson ◽  
D Aoude-Werner ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Vitamin C ◽  
Infant Formula ◽  
Collaborative Study ◽  
Uv Detection ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility

Abstract To determine the repeatability and reproducibility values of the AOAC INTERNATIONAL First Action Method 2012.22, Vitamin C in Infant Formula and Adult/Pediatric Nutritional Formula by Liquid Chromatography with UV Detection, a collaborative study was organized The study was dividedinto two parts: method setup and qualification of participants (part 1) and collaborative study participation (part 2). During part 1, each laboratory was asked to analyze two practice samples using the aforementioned method Laboratories that provided results within a range of expected levels were qualified for part 2, where they analyzed 10 samples in blind duplicates Two of the samples were suspected of spoilage during the test and new cans of the same type of product were analyzed by a subset of laboratories in part 3. The results were compared with Standard Method Performance Requirement (SMPR®) 2012.012 established for vitamin C The precision results were within the requirements stated in the SMPR: 1.4–7.3% and 3.2–11.4% respectively, for repeatability and reproducibility Finally, Horwitz ratio values were all <2 (0.5–1.7). The Expert Review Panel for Stakeholder Panel for Infant Formula and Adult Nutritionals Nutrient Methods determined that the data presented met the SMPR and therefore recommended the method be granted Final Action status.

Determination of Sodium Fluoroacetate in Dairy Powders by Liquid Chromatography–Tandem Mass Spectrometry: Single-Laboratory Validation, First Action 2015.02

2016 ◽  
Vol 99 (1) ◽  
pp. 242-251 ◽  
Author(s):  
Lauren M Fleury ◽  
Bryan G Scahill ◽  
Rilka Taskova
Keyword(s):  
Infant Formula ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Liquid Chromatography Tandem Mass ◽  
Expert Review Panel ◽  
Single Laboratory ◽  
Lc Tandem Ms ◽  
Dairy Powders

Abstract A single-laboratory validation (SLV) study was conducted for the determination of sodium fluoroacetate in dairy powders by LC-tandem MS (LC-MS/MS). Linearity of response was confirmed by analysis of samples fortified over the concentration range 0.10–100 μg/kg. The LOD was estimated to be 0.028 μg/kg (0.028 ppb) from the SD of the measured concentrations of infant formula samples fortified at 0.10 μg/kg. The corresponding LOQ calculates at 0.085 μg/kg (0.085 ppb), which ensures excellent reliability of quantification at the limit of reporting of 1.0 μg/kg (1 ppb). Repeatability and intermediate precision were estimated from the SD of the recovery of samples fortified at 0.075, 0.10, 0.20, 0.50, 1.0, and 10.0 μg/kg. The previously mentioned method performance values were established using a representative stage 2 (6–12 months) bovine infant formula, and the robustness of the method was tested by the analysis of 107 unique dairy powders and formulations fortified at 1.0 μg/kg. The data collected in this study satisfy the requirements of SLV studies established by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN), and the method was awarded First Action Official MethodSM status by the AOAC Expert Review Panel on SPIFAN Nutrient Methods (Contaminants) on March 17, 2015.

scholarly journals Total Amino Acids by UHPLC–UV in Infant Formulas and Adult Nutritionals, First Action 2018.06

2019 ◽  
Vol 102 (5) ◽  
pp. 1574-1588 ◽  
Author(s):  
Greg Jaudzems ◽  
Joseph Guthrie ◽  
Sabine Lahrichi ◽  
Christophe Fuerer
Keyword(s):  
Amino Acids ◽  
Infant Formula ◽  
Amino Acid Content ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Single Laboratory ◽  
Total Amino Acids

Abstract 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.

Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation: A Multilaboratory Testing Study, Final Action 2011.06

2018 ◽  
Vol 101 (6) ◽  
pp. 1881-1894 ◽  
Author(s):  
Sneh D Bhandari ◽  
Ming Gao ◽  
John Szpylka ◽  
N Collopy ◽  
H Chen ◽  
...  
Keyword(s):  
Infant Formula ◽  
Collaborative Study ◽  
Reference Method ◽  
Official Method ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Relative Standard ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility

Abstract Background: The need for an updated reference method for folate was identified as a priority by the AOAC’s Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) in 2011. An Expert Review Panel (ERP) found AOAC Official MethodSM 2011.06 suitable for the purpose and approved it as a First Action Official Method. Objective: To determine the repeatability and reproducibility of Method 2011.06: Total Folate in Infant Formula and Adult Nutritionals by Trienzyme Extraction and LC-MS/MS Quantitation. Methods: A multilaboratory collaborative study was conducted. Eleven laboratories located in five countries participated and completed analysis of all multilaboratory testing (MLT) samples. The study was divided into two parts. In the first part, the laboratories analyzed two practice samples (blindly coded) using the updated folate Method 2011.06. The laboratories providing results within the expected range qualified for part two, in which they analyzed 11 MLT samples in blind duplicates. Results: The results were compared with the Standard Method Performance Requirements (SMPR 2011.006) established for folate. The precision results met the requirements stated in the SMPR for all of the samples. Repeatability and reproducibility relative standard deviations ranged from 3.5 to 6.6 and from 9.0 to 15.7%, respectively. Horwitz ratio values for all of the samples were well below 2 (0.61–1.06). Conclusions: The ERP determined that the method performance met the SMPR requirements in September 2017 after reviewing the presented MLT data. Highlights: The ERP recommended the method for Final Action status.

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