scholarly journals Vitamin B12 (cyanocobalamin) in Infant Formula Adult/Pediatric Nutritional Formula by Liquid Chromatography with Ultraviolet Detection: Collaborative Study, Final Action 2014.02

2018 ◽  
Vol 101 (4) ◽  
pp. 1112-1118 ◽  
Author(s):  
Ester Campos Giménez ◽  
Frédéric Martin ◽  
F Arella ◽  
J Austad ◽  
S Bandhari ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Vitamin B12 ◽  
Infant Formula ◽  
Collaborative Study ◽  
Review Panel ◽  
Expert Review ◽  
Relative Standard ◽  
Two Samples ◽  
Expert Review Panel ◽  
Repeatability And Reproducibility

Abstract To determine the repeatability and reproducibility figures of the AOAC First Action Official MethodSM 2014.02 (Vitamin B12 in Infant Formula and Adult/Pediatric Formula by Liquid Chromatography with UV Detection), a collaborative study was organized. Twenty-one laboratories located in 13 different countries agreed to participate. The study was divided into two parts. During the first part, the laboratories analyzed two samples in duplicate by using the method described in the protocol. The laboratories that provided results within the expected range were qualified for part two, during which they analyzed 10 samples in blind duplicates. Eighteen laboratories managed to provide results on time for reporting. The results were compared with the Standard Method Performance Requirement (SMPR® 2011.005) established for vitamin B12. The precision results met the requirements stated in the SMPR except for one sample. Repeatability and reproducibility relative standard deviation ranged from 1.1 to 6.5% and from 6.0 to 23.8%, respectively, with only one matrix showing reproducibility values higher than the required 11%. Horwitz ratio values were all well below 2 (0.17–0.78). The AOAC Expert Review Panel (Stakeholder Panel for Infant Formula and Adult Nutritional Expert Review Panel) determined that the data presented met the SMPR and, hence, recommended the method to be granted Final Action status in September 2016.

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.

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.

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.

Determination of Vitamin B12 in Infant Formula and Adult Nutritionals by Liquid Chromatography/UV Detection with Immunoaffinity Extraction: First Action 2011.08

2012 ◽  
Vol 95 (2) ◽  
pp. 307-312 ◽  
Author(s):  
Esther Campos-Giménez ◽  
Patric Fontannaz ◽  
Marie-José Trisconi ◽  
Tamara Kilinc ◽  
Catherine Gimenez ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Vitamin B12 ◽  
Infant Formula ◽  
Uv Detection ◽  
Infant Formulas ◽  
Method Performance ◽  
Expert Review ◽  
Expert Review Panel ◽  
C 30

Abstract At the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting,” on June 29, 2011, an Expert Review Panel agreed that the method “Determination of Vitamin B12 in Infant Formulas and Adult Nutritionals by Liquid Chromatography/UV Detection with Immunoaffinity Extraction” be adopted AOAC Official First Action status. The method is applicable for the determination of vitamin B12, which includes added cyanocobalamin and natural forms, making it applicable to both fortified and nonfortified products. Vitamin B12 is extracted from the sample in sodium acetate buffer in the presence of sodium cyanide (100°C, 30 min). After purification and concentration with an immunoaffinity column, vitamin B12 is determined by LC with UV detection (361 nm). A single-laboratory validation study was conducted on a range of products, including milk- and soy-based infant formulas, cereals, cocoa beverages, health care products, and polyvitamin premixes. The method demonstrated linear response over a large range of concentrations, recovery rates of 100.8 ± 7.5% (average ± SD), repeatability RSD (RSDr) of 2.1%, and intermediate reproducibility (RSDiR) of 4.3%. LOD and LOQ values were 0.10 and 0.30 μg/100 g, respectively, and correlation with the reference microbiological assay was good (R2 = 0.9442). The results of the study were published in J. AOAC Int. 91, 786–793 (2008). The performance characteristics of the method met the standard method performance requirements set forth by the Stakeholder Panel on Infant Formula and Adult Nutritionals; thus, the method was determined to be appropriate for First Action status.

Determination of Vitamin B12 in Infant Formula and Adult Nutritionals by HPLC: First Action 2011.10

2012 ◽  
Vol 95 (2) ◽  
pp. 313-318 ◽  
Author(s):  
Karen Schimpf ◽  
Renee Spiegel ◽  
Linda Thompson ◽  
Dawn Dowell
Keyword(s):  
Vitamin B12 ◽  
Infant Formula ◽  
Review Panel ◽  
Intermediate Precision ◽  
Expert Review ◽  
Quantitation Limit ◽  
Expert Review Panel ◽  
Analytical Range ◽  
Standard Range

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) reviewed the method “Determination of Vitamin B12 in Infant Formula and Adult Nutritionals by HPLC.” Under the new pathway to Official MethodsSM, the ERP adopted the method as Official First Action. The method is applicable to the determination of vitamin B12 in infant formula and adult nutritionals. Data showed an average overall intermediate precision of 6.64% RSD, an estimated quantitation limit of 0.8 μg/kg, and a detection limit of 0.2 μg/kg in prepared samples. The standard range of the method is 2 to 200 μg/L, which corresponds to an analytical range of 0.8 to 500 μg/kg.

scholarly journals Determination of Aflatoxin B1 in Baby Food (Infant Formula) by Immunoaffinity Column Cleanup Liquid Chromatography with Postcolumn Bromination: Collaborative Study

2001 ◽  
Vol 84 (4) ◽  
pp. 1116-1124 ◽  
Author(s):  
Joerg Stroka ◽  
Elke Anklam ◽  
Urban Joerissen ◽  
John Gilbert ◽  
A Barmark ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Infant Formula ◽  
Aflatoxin B1 ◽  
Collaborative Study ◽  
Baby Food ◽  
Immunoaffinity Column ◽  
Relative Standard

Abstract A collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for determination of aflatoxin B1 in a milk powder based infant formula at a possible future European regulatory limit (0.1 ng/g). The test portion was extracted with methanol–water (8 + 2 [v + v]), filtered, diluted with water, and applied to an immunoaffinity column. The column was washed with water to remove interfering compounds, and the purified aflatoxin B1 was eluted with methanol. The separation and determination of the aflatoxin B1 was performed by reversed-phase LC and detected by fluorescence after postcolumn derivatization (PCD) involving bromination. PCD was achieved with either pyridinum hydrobromide perbromide (PBPB) or an electrochemical (Kobra) cell by addition of bromide to the mobile phase. The baby food (infant formula) test samples, both spiked and naturally contaminated with aflatoxin B1, were sent to 14 laboratories in 13 different European countries. Test portions were spiked at levels of 0.1 and 0.2 ng/g for aflatoxin B1. Recoveries ranged from 101 to 92%. Based on results for spiked test samples (blind pairs at 2 levels) and naturally contaminated test samples (blind pairs at 3 levels), the relative standard deviation for repeatability (RSDr) ranged from 3.5 to 14%. The relative standard deviation for reproducibility (RSDR) ranged from 9 to 23%. Nine participants used PBPB derivatization, and 5 particpants used the Kobra cell. There was no evidence of method performance depending on the derivatization method used. The method showed acceptable within- and between-laboratory precision for baby food matrix, as evidenced by HORRAT values, at the target levels of determination for aflatoxin B1.

Determination of Vitamin B12 in Infant, Adult, and Pediatric Formulas by HPLC-UV and Column Switching: Collaborative Study, Final Action 2011.10

2015 ◽  
Vol 98 (6) ◽  
pp. 1655-1665 ◽  
Author(s):  
Linda D Butler-Thompson ◽  
Wesley A Jacobs ◽  
Karen J Schimpf ◽  
J Austad ◽  
B Chen ◽  
...  
Keyword(s):  
Vitamin B12 ◽  
Collaborative Study ◽  
Potassium Cyanide ◽  
Column Switching ◽  
Biologically Active ◽  
Size Exclusion ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel

Abstract AOAC First Action Method 2011.10, Vitamin B12 in Infant and Pediatric Formulas and Adult Nutritionals, was collaboratively studied. This method uses a pH 4.5 sodium acetate buffer and potassium cyanide at 105°C to extract and convert all biologically active forms of vitamin B12 present to cyanocobalamin; octylsilyl (C8) or C18 SPE cartridges to purify and concentrate cyanocobalamin; a combination of size-exclusion and RPLC to isolate cyanocobalamin; and visible absorbance at 550 nm to detect and quantitate cyanocobalamin in infant, pediatric, and adult nutritionals with vitamin B12 concentrations greater than 0.025 μg/100 g ready-to-feed (RTF) liquid. During this collaborative study, nine to 11 laboratories from eight different countries analyzed blind duplicates of 12 infant, pediatric, and adult nutritional formulas. Per the AOAC Expert Review Panel (ERP) on Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Nutrient Methods the method demonstrated acceptable repeatability and reproducibility and met SPIFAN Standard Method Performance Requirements (SMPRs®) for the majority of product matrixes analyzed. Vitamin B12 SPIFAN SMPRs for repeatability were ≤15% RSD at vitamin B12 concentrations of 0.01 μg/100 g RTF liquid and ≤7% RSD at vitamin B12 concentrations of 0.2–5.0 μg/100 g RTF liquid. Vitamin B12 SPIFAN SMPRs for reproducibility were ≤11% RSD in products with vitamin B12 concentrations ranging from 0.3 to 5.0 μg/100 g RTF liquid. During this collaborative study, the RSDr ranged from 2.98 to 9.77%, and the RSDR ranged from 3.54 to 19.5%. During previous single-laboratory validation studies, the method LOQ was estimated to be 0.025 μg/100 g RTF liquid.

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.

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.

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