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.

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.

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.

Determination of Vitamin B12 in Infant Formula and Adult Nutritionals Using HPLC After Purification on an Immunoaffinity Column: First Action 2011.09

2012 ◽  
Vol 95 (4) ◽  
pp. 933-936 ◽  
Author(s):  
Ursula Kirchner ◽  
Katharina Degenhardt ◽  
Guenther Raffler ◽  
Maria Nelson
Keyword(s):  
Vitamin B12 ◽  
Measurement Uncertainty ◽  
Infant Formula ◽  
Potassium Cyanide ◽  
Immunoaffinity Column ◽  
Validation Data ◽  
Method Performance ◽  
Expert Review ◽  
Wide Range

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting,” on June 29, 2011, the method “Determination of Vitamin B12 in Infant Formula and Adult Nutritionals Using HPLC After Purification on an Immunoaffinity Column” was recommended by an Expert Review Panel and adopted as AOAC Official First Action status. The method is applicable for the determination of vitamin B12 in milk-based infant formula. Vitamin B12 is extracted from the sample in sodium acetate buffer in the presence of potassium cyanide. After purification and concentration with an immunoaffinity column (IAC), vitamin B12 is determined by LC with UV detection (361 nm). Data supplied by CLF demonstrated linear response over a wide range of concentrations (1.4–39 μg/100 mL). The analytical range is 0.2–10 μg/100 g, depending on the capacity of the IACs (0.01–0.5 μg), the input weight, and dilutions. Recovery rates were assessed using National Institute of Standards and Technology SRM 1849, and determined to be 95.1%, with SD of 0.34 and CV of 9.0. Measurement uncertainty (UE) was 0.8 μg/100 g, which was calculated from the validation data. It is an expanded measurement uncertainty and was obtained through multiplication with a coverage factor k. LOQ values were reported as 0.10 μg/100 g. The performance characteristics of the method met the standard method performance requirements set forth by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals; thus, the method was determined to be appropriate for First Action status.

Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals: First Action 2011.13

2012 ◽  
Vol 95 (3) ◽  
pp. 583-587 ◽  
Author(s):  
Donald L Gilliland ◽  
Charles K Black ◽  
James E Denison ◽  
Charles T Seipelt ◽  
Dawn Dowell
Keyword(s):  
Simultaneous Determination ◽  
Infant Formula ◽  
Practical Method ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Working Standards

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) on behalf of AOAC INTERNATIONAL adopted the method “Simultaneous Determination of Vitamins D2 and D3 by LC-MS/MS in Infant Formula and Adult Nutritionals” as an AOAC Official First Action method. Vitamins D2 and D3 are extracted from the sample using pentane–ether; the extract is collected and dried under nitrogen. Vitamin D is separated from interfering compounds using UPLC, and quantitated using tandem mass spectrometry (MS/MS). Preliminary data showed the intermediate precision ranged from 3.34–8.05% and an accuracy range of 98.5–111% over the samples tested for vitamin D3. For vitamin D2, the intermediate precision ranged from 2.37–5.45% and accuracy ranged from 96.4–104% over the four matrixes evaluated. The analytical range for the method is bounded by the concentrations of the working standards, 21–270 ng/mL, and is equivalent to 0.168–2.16 mcg/100 g in ready-to-feed product. The practical method quantitation limit is 0.168 mcg/100 g product with method detection limit of 60 ng/100 g product. The ERP reviewed the data and determined that the performance characteristics of the method met the standard method performance requirements, and therefore the method was granted First Action status.

Choline in Infant Formula and Adult Nutritionals by Ion Chromatography and Suppressed Conductivity: First Action 2012.20

2013 ◽  
Vol 96 (6) ◽  
pp. 1400-1406 ◽  
Author(s):  
Kassandra Oates ◽  
Lillian Chen ◽  
Brian De Borba ◽  
Deepali Mohindra ◽  
Jeffrey Rohrer ◽  
...  
Keyword(s):  
Infant Formula ◽  
Ion Chromatography ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Technology Standard ◽  
Expert Review Panel ◽  
Suppressed Conductivity Detection ◽  
Single Laboratory

Abstract Single-laboratory validation (SLV) data from a method for the determination of choline in infant formula and adult nutritionals by ion chromatography (IC) and suppressed conductivity were generated and presented to the Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Expert Review Panel (ERP) at the AOAC Annual Meeting held in Las Vegas, NV, during September 30 to October 3, 2012. The ERP reviewed the data and concluded that the data met the standard method performance requirements (SMPRs) established and approved the method as AOAC Official First Action. At the ERP's request, a second, full SLV was performed on 17 SPIFAN matrixes that included fortified and placebo products. Prior to IC analysis, microwave-assisted acid hydrolysis was used to digest and release bound choline from powder and ready-to-feed (RTF) infant formula and adult nutritional samples. Following hydrolysis, separation of choline from common cations was achieved on a Thermo ScientificTM DionexTM IonPacTM CS19 column followed by suppressed conductivity detection. Total choline was measured and reported as the choline ion in mg/100 g reconstituted material or RTF as-is. The system was calibrated over the analytical range specified in the SMPR (2–250 mg/100 g). Recoveries of spiked samples at 50 and 100% of the fortified choline amounts ranged from 93.1 to 100.7% with RSDs ≤6.7% for product containing <2 mg/100 g and ≤4.1% for product containing 2–100 mg/100 g. Accuracy for the National Institute of Standards and Technology Standard Reference Material 1849a was determined over a 6-day interval and found to be 10.2 ± 0.2 mg/100 g calculated as the reconstituted powder with an RSD of 1.8%. The LOD was determined to be 0.009, and the LOQ 0.012 mg/100 g, well below the SMPR requirements of 0.7 and 2 mg/100 g, respectively. Repeatability RSDs over the range of the assay (2–200 mg/100 g) ranged from 1.0 to 5.93%

Determination of Chloride in Infant Formula and Adult/Pediatric Nutritional Formula by Automated Potentiometry: Single-Laboratory Validation, First Action 2015.08

2015 ◽  
Vol 98 (5) ◽  
pp. 1390-1394
Author(s):  
Gregory G Jaudzems
Keyword(s):  
Infant Formula ◽  
Nitrate Solution ◽  
Chloride Content ◽  
Silver Nitrate Solution ◽  
Intermediate Precision ◽  
Method Performance ◽  
Expert Review ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A direct potentiometric method involving titration against a standard volumetric silver nitrate solution using a silver electrode to detect the end point was evaluated for the determination of chloride in infant formula and adult/pediatric nutritional formula. It was assessed for compliance against AOAC Standard Method Performance Requirements (SMPR®) established by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN). A single-laboratory validation (SLV) study was conducted as a first step in the process to validate the method. In this SLV, 17 SPIFAN matrixes representing a range of infant formula and adult nutritional products were evaluated for their chloride content. The analytical range was found to be between 1.4 and 1060 mg/100 g reconstituted product or ready-to-feed (RTF) liquid. The LOQ was estimated as 1.4 mg/100 g. Method repeatability was between 0.03 and 1.60% in the range of 20 to 167 mg/100 g RTF, and intermediate precision was between 0.09 and 2.77% in the same range. Recovery values based on spiking experiments at two different levels of chloride ranged from 99.0 to 103% for 15 different SPIFAN products. Evaluation of trueness was performed on National Institute of Standards and Technology Standard Reference Material 1849a (Infant/Adult Nutritional Formula) and showed 97.2% of the theoretical value, with no bias at the 95% confidence level. Based on the results of the SLV, the method met the SMPR and was approved as a First Action method by the AOAC Expert Review Panel on Infant Formula and Adult Nutritionals on March 17, 2015.

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.

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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