Determination of Folate in Infant Formula and Adult/Pediatric Nutritional Formula by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry: First Action 2013.13

2014 ◽  
Vol 97 (4) ◽  
pp. 1121-1126 ◽  
Author(s):  
Karine Meisser-Redeuil ◽  
Sylvie Bénet ◽  
Catherine Gimenez ◽  
Esther Campos-Giménez ◽  
Maria Nelson
Keyword(s):  
Folic Acid ◽  
Infant Formula ◽  
High Performance ◽  
Intermediate Precision ◽  
Method Performance ◽  
Performance Requirements ◽  
Vitamin B9 ◽  
Target Values ◽  
Liquid Chromatography Tandem Mass

Abstract A UHPLC-MS/MS method for the determination of folate (vitamin B9) in infant formula and adult/pediatric nutritional formula was assessed for compliance with standard method performance requirements set forth by the AOAC INTERNATIONAL Stakeholder Panel for Infant Formula and Adult Nutritionals (SPIFAN). A single-laboratory validation (SLV) study was conducted as the first step in the process to validate the method. In the study, 12 matrixes, representing the range of infant and adult nutritional products, were evaluated for folate [the sum of supplemental folic acid plus 5-methyl tetrahydrofolic acid (5-Me THF)]. Method response was linear in the range of 1.0–900 ng/mL, corresponding to 0.33–300 μg/100 g in reconstituted sample. LOD for folic acid and 5-Me THF, expressed in reconstituted product, were 0.10 μg/100 g and 0.05 μg/100 g, respectively, and LOQ were 0.33 μg/100 g and 0.10 μg/100 g, respectively. Repeatability was <5.3% and intermediate precision was <5.5%. Recovery rates of spiking at 50 and 100% of target values in nonfortified products were within 90–110%. Evaluation of trueness was performed on Certified Reference Material (SRM 1849 Infant/Adult Nutritional Formula) and gave 96.4% of theoretical value. Based on the results of the SLV, the method meets the SPIFAN requirements for AOAC First Action status for the determination of folates in infant formula and adult/pediatric nutritional formula.

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.

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.

Determination of Lutein and β-Carotene in Infant Formula and Adult Nutritionals by Ultra-High-Performance Liquid Chromatography: Single-Laboratory Validation, First Action 2016.13

2017 ◽  
Vol 100 (3) ◽  
pp. 768-781
Author(s):  
Gregory L Hostetler
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Infant Formula ◽  
High Performance ◽  
Hplc Method ◽  
Method Performance ◽  
Performance Requirements ◽  
Single Laboratory ◽  
Β Carotene

Abstract An ultra-HPLC method for the determination of lutein and β-carotene in infant formula and adult nutritionals wasvalidated using both unfortified and fortified samples provided by the AOAC Stakeholder Panel on Infant Formula and AdultNutritionals (SPIFAN). All experiments showed separation of all-trans-lutein and β-carotene from their major cis isomers, apocarotenal, α-carotene, lycopene, and zeaxanthin. Samples spiked with all-trans-lutein and β-carotene showed no isomerization during sample preparation. Linearity of the calibration solutions correlated to approximately 0.8–45 μg/100 g (reconstituted basis) for samples prepared for the lowest sample concentrations. With dilutions specified in the method, the range can be extended to approximately 2250 μg/100 g. The LOD for both lutein and β-carotene was 0.08 μg/100 g, and the LOQ for both was 0.27μg/100 g. For all measurements in the range of 1–100 μg/100 g, repeatability RSD was ≤5.8% forlutein and ≤5.1% for β-carotene. For measurements >100 μg/100 g, repeatability RSD was ≤1.1% for lutein and ≤1.7% for β-carotene. Accuracywas determined by recovery from spiked samples and ranged from 92.3 to 105.5% for lutein and from 100.1 to 107.5% for β-carotene. The data provided show that the method meets the criteria specified in the Standard Method Performance Requirements for carotenoids (SMPR 2014.014).

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.

Determination of Lutein, β-Carotene, and Lycopene in Infant Formula and Adult Nutritionals by Ultra-High Performance Liquid Chromatography: Collaborative Study, Final Action 2016.13 for β-Carotene and Lycopene Only

2020 ◽  
Vol 103 (3) ◽  
pp. 818-832
Author(s):  
Gregory L Hostetler ◽  
S Benét ◽  
R Buis ◽  
E Campos-Giménez ◽  
S Christiansen ◽  
...  
Keyword(s):  
Infant Formula ◽  
High Performance ◽  
Collaborative Study ◽  
Method Performance ◽  
Performance Requirements ◽  
Repeatability And Reproducibility ◽  
Aoac Official ◽  
Sample Set ◽  
Β Carotene

Abstract Background Lutein, β-carotene, and lycopene are among the most common carotenoids present in human milk and are frequently added to infant formula and adult nutritionals. Objective A collaborative study was conducted to assess the interlaboratory performance of AOAC Official MethodSM2016.13 for the determination of lutein, β-carotene, and lycopene in infant formula and adult nutritionals. Methods Thirteen laboratories agreed to participate in the study and 10 laboratories from seven different countries reported results. The study samples included blind duplicates of 6 matrices fortified with lutein, 7 matrices fortified with β-carotene, and 1 fortified with lycopene. NIST SRM 1869 was included in the sample set as a reference material. Results After the removal of outliers and invalid data, the repeatability (RSDr) data was ≤10.0% for all-trans-lutein, ≤12.0% for total lutein, ≤4.2% for all-trans-β-carotene, ≤6.0% for total β-carotene, and 1.6% for total lycopene. Reproducibility (RSDR) was ≤14.8% for all-trans-lutein, ≤19.9% for total lutein, ≤15.3% for all-trans-β-carotene, ≤13.7% for total β-carotene, and 7.4% for total lycopene. Conclusions The repeatability and reproducibility values met the criteria in the Standard Method Performance Requirements (SMPRs) for β-carotene and lycopene and it was recommended that the method be approved as a Final Action for these analytes. Since the method did not meet the SMPR for lutein, it was recommended that it remain a First Action method for this analyte. Highlights AOAC Official MethodSM2016.13 was validated through a collaborative study to be accurate and reproducible for the determination of β-carotene and lycopene in infant formula and adult nutritionals.

scholarly journals Determination of Chondroitin Sulfate Content in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography with UV Detection After Enzymatic Hydrolysis: Single-Laboratory Validation First Action 2015.11

2016 ◽  
Vol 99 (1) ◽  
pp. 53-54
Author(s):  
Sharon L Brunelle
Keyword(s):  
Chondroitin Sulfate ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A previously validated method for determination of chondroitin sulfate in raw materials and dietary supplements was submitted to the AOAC Expert Review Panel (ERP) for Stakeholder Panel on Dietary Supplements Set 1 Ingredients (Anthocyanins, Chondroitin, and PDE5 Inhibitors) for consideration of First Action Official MethodsSM status. The ERP evaluated the single-laboratory validation results against AOAC Standard Method Performance Requirements 2014.009. With recoveries of 100.8–101.6% in raw materials and 105.4–105.8% in finished products and precision of 0.25–1.8% RSDr within-day and 1.6–4.72% RSDr overall, the ERP adopted the method for First Action Official Methods status and provided recommendations for achieving Final Action status.

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.

Determination of Vitamin K1 in Infant, Pediatric, and Adult Nutritionals by HPLC with Fluorescence Detection: Single-Laboratory Validation, First Action 2015.09

2015 ◽  
Vol 98 (5) ◽  
pp. 1382-1389 ◽  
Author(s):  
Mary Bidlack ◽  
Linda D Butler Thompson ◽  
Wesley A Jacobs ◽  
Karen J Schimpf
Keyword(s):  
Fluorescence Detection ◽  
Hplc Method ◽  
Excitation Wavelength ◽  
Vitamin K1 ◽  
Intermediate Precision ◽  
Method Performance ◽  
Performance Requirements ◽  
Normal Phase Hplc ◽  
Single Laboratory

Abstract This normal-phase HPLC method with postcolumn reduction and fluorescence detection allows for the quantitative determination of trans vitamin K1 in infant, pediatric, and adult nutritionals. Vitamin K1 is extracted from products with iso-octane after precipitation of proteins and release of lipids with methanol. Prepared samples are injected onto a silica HPLC column where cis and trans vitamin K1 are separated with an iso-octane–isopropanol mobile phase. The column eluent is mixed with a dilute ethanolic solution of zinc chloride, sodium acetate, and acetic acid, and vitamin K1 is reduced to a fluorescent derivative in a zinc reactor column. The resulting hydroquinone is then detected by fluorescence at an excitation wavelength of 245 nm and an emission wavelength of 440 nm. During a single-laboratory validation of this method, repeatability and intermediate precision ranged from 0.6 to 3.5% RSD and 1.1 to 6.0% RSD, respectively. Mean overspike recoveries ranged from 91.9 to 106%. The method demonstrated good linearity over a standard range of approximately 2–90 μg/L trans vitamin K1 with r2 averaging 0.99995 and average calibration errors of <1%. LOQ and LOD in ready-to-feed nutritionals were estimated to be 0.03 and 0.09 μg/100 g, respectively. The method met AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals Standard Method Performance Requirements® and was approved as a first action method at the 2015 AOAC Mid-Year Meeting.

Determination of Fructans in Infant, Adult, and Pediatric Nutritional Formulas: Single-Laboratory Validation, First Action 2016.06

2016 ◽  
Vol 99 (6) ◽  
pp. 1576-1588 ◽  
Author(s):  
Philip Haselberger ◽  
Wesley A Jacobs
Keyword(s):  
Quantitative Analysis ◽  
Sample Preparation ◽  
Profile Analysis ◽  
Correction Factors ◽  
Intermediate Precision ◽  
Size Category ◽  
Method Performance ◽  
Performance Requirements ◽  
Single Laboratory

Abstract A method for fructan analysis designed to comply with AOAC Standard Method Performance Requirements (SMPR®) 2014.002 is described. It is closely related to existing methods for fructan analysis, including AOAC 997.08 and 999.03, as well as a method previously published by Cuany et al. This new method achieves LOQ of 0.03% fructan on a ready-to-feed (RTF) basis with mean recoveries ranging from 93 to 108% in the presence of up to 9% sucrose (even at the 0.03% level of fructan). Repeatability ranged from 1.09 to 3.67%. Intermediate precision ranged from 2.46 to 6.79%. Sample preparation for quantitative analysis is simplified compared to some of the existing methodologies. The method incorporates a qualitative profile analysis to determine fructan size category. This allows assignment of appropriate correction factors without independent knowledge of fructan type.

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