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.

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).

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 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.

Determination of Myo-Inositol in Infant, Pediatric, and Adult Formulas by Liquid Chromatography-Pulsed Amperometric Detection with Column Switching: Collaborative Study, Final Action 2011.18

2015 ◽  
Vol 98 (6) ◽  
pp. 1666-1678 ◽  
Author(s):  
Linda D Butler-Thompson ◽  
Wesley A Jacobs ◽  
Karen J Schimpf ◽  
J Austad ◽  
L Basumallick ◽  
...  
Keyword(s):  
Gold Electrode ◽  
Dilute Hydrochloric Acid ◽  
Collaborative Study ◽  
Amperometric Detection ◽  
Column Switching ◽  
Glycerol Backbone ◽  
Method Performance ◽  
Performance Requirements ◽  
Repeatability And Reproducibility

Abstract AOAC First Action Method 2011.18, Myo-Inositol (Free and Bound as Phosphatidylinositol) in Infant and Pediatric Formulas and Adult Nutritionals, was collaboratively studied. With this method free myo-inositol and phosphatidylinositol bound myo-inositol are extracted using two different sample preparation procedures, separated by ion chromatography using a combination of Dionex Carbo Pac PA1 and MA1 columns with column switching, and detected with pulsed amperometry using a gold electrode. Free myo-inositol is extracted from samples with dilute hydrochloric acid and water. Phosphatidylinositol is extracted from samples with chloroform and separated from other fats with silica SPE cartridges. Myo-inositol is then released from the glycerol backbone with concentrated acetic and hydrochloric acids at 120°C. During this collaborative study, nine laboratories from five different countries analyzed blind duplicates of nine infant and pediatric nutritional formulas for both free and phosphatidylinositol bound myo-inositol, and one additional laboratory only completed the free myo-inositol analyses. The method demonstrated acceptable repeatability and reproducibility and met the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Standard Method Performance Requirements (SMPRs®) for free myo-inositol plus phosphatidylinositol bound myo-inositol for all the matrixes analyzed. SMPRs for repeatability were ≤5% RSD at myo-inositol concentrations of 2–68 mg/100 g ready-to-feed (RTF) liquid. SMPRs for reproducibility were ≤8% RSD in products with myo-inositol concentrations ranging from 2 to 68 mg/100 g RTF liquid. During this collaborative study, repeatability RSDs ranged from 0.51 to 3.22%, and RSDs ranged from 2.66 to 7.55% for free myo-inositol plus phosphatidylinositol bound myo-inositol.

Determination of trans and Total Vitamin K1 in Infant, Pediatric, and Adult Nutritionals by HPLC with Post Column Reduction and Fluorescence Detection: Multilaboratory Testing Study, AOAC Final Action 2015.09

2019 ◽  
Vol 102 (1) ◽  
pp. 222-232
Author(s):  
Karen J Schimpf ◽  
Linda D Butler Thompson ◽  
Shang-Jing Pan ◽  
P Delmonte ◽  
C Domer ◽  
...  
Keyword(s):  
Infant Formula ◽  
Fluorescence Detection ◽  
Vitamin K1 ◽  
Method Performance ◽  
Performance Requirements ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Cis And Trans ◽  
Fluorescent Derivatives

Abstract A multilaboratory study was completed with AOAC INTERNATIONAL First Action Official MethodSM 2015.09, “Determination of trans and Total (cis+trans) Vitamin K1 in Infant, Pediatric, and Adult Nutritionals by HPLC with Post Column Reduction and Fluorescence Detection.” Eight laboratories from six countries participated in the multilaboratory study. Each laboratory analyzed 19 infant, pediatric, and adult nutritionals in duplicate. The product matrixes analyzed included milk, soy, partially hydrolyzed milk, partially hydrolyzed soy, and elemental-based infant formula powders; milk-based infant formula ready-to-feed liquids; pediatric powders; adult low- and high-fat powders; and high-protein ready-to-drink nutritionals. Vitamin K1 was extracted from product matrixes with isooctane after precipitation of proteins and the release of lipids with methanol. Prepared samples were injected onto a silica HPLC column in which cis and trans vitamin K1 were separated with an isooctane–isopropanol mobile phase. The column eluent was mixed with a dilute ethanolic solution of zinc chloride, sodium acetate, and acetic acid, and cis and trans vitamin K1 were reduced to fluorescent derivatives in a zinc reactor column. Overall, trans vitamin K1 repeatability averaged 3.06% relative standard deviation (RSD) with a range of 0.99–7.16% RSD and reproducibility averaged 6.36% RSD with a range of 3.15–16.1% RSD. Repeatability Standard Method Performance Requirements (SMPR®) were met for all 19 matrixes, and reproducibility SMPRs were met for 18 of the 19 product matrixes analyzed. Repeatability and reproducibility for total (cis + trans) vitamin K1 averaged 3.15% RSD with a range of 1.06–6.87% RSD and 6.11% RSD with a range of 2.94–16.7% RSD, respectively.

Determination of Fructans in Infant Formula and Adult/Pediatric Nutritional Formula by Anion-Exchange Chromatography with Pulsed Amperometric Detection after Enzymatic Treatment: Collaborative Study, Final Action 2016.14

2020 ◽  
Vol 103 (5) ◽  
pp. 1301-1317
Author(s):  
Véronique Spichtig ◽  
Sean Austin ◽  
Kommer Brunt ◽  
Jeroen Van Soest ◽  
Peter Sanders
Keyword(s):  
Infant Formula ◽  
Collaborative Study ◽  
Amperometric Detection ◽  
Anion Exchange Chromatography ◽  
Exchange Chromatography ◽  
Method Performance ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel

Abstract Background Fructans are added to infant formula and adult nutritionals for their prebiotic effect. A method (AOAC 2016.14) was developed for their analysis which has already demonstrated excellent performance during single laboratory validation. Objective To determine repeatability and reproducibility of the method through a collaborative study. Methods Fourteen laboratories from 11 different countries enrolled for the study. Participants analyzed a practice sample, then 8 formula or adult nutritionals in blind duplicate. Results and any method modifications were reported to the study director. Results Twelve laboratories provided results on time for reporting. Precision results for five samples met the requirements of the Standard Method Performance Requirements (SMPR 2014.002), with RSDr ranging from 3.60 to 4.25% and RSDR ranging from 5.90 to 11.7%. The practice sample also met the requirements of SMPR 2014.002, with RSDr and RSDR of 2.53% and 6.70% respectively. Precision results for three test samples did not fully meet the SMPR, with RSDr ranging from 2.27 to 7.65% and RSDR ranging from 12.8 to 15.1%. After review, the AOAC Stakeholder Panel for Infant Formula and Adult Nutritional Expert Review Panel (SPIFAN ERP) concluded that the data presented mostly met the SMPR and hence recommended that the method to be advanced for adoption as an AOAC Final Action method. Conclusions The method described in AOAC 2016.14 is suitable for the determination of fructans in infant formula and adult nutritionals.

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.

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.

AOAC SMPR® 2017.006:Standard Method Performance Requirements (SMPRs) for Determination of β-Carotene in Infant and Adult/ Pediatric Nutritional Formula

2017 ◽  
Vol 100 (4) ◽  
pp. 1217-1218
Author(s):  
Gregory Hostetler ◽  
Sneh Bhandari ◽  
Carolyn Burdette ◽  
Adrienne McMahon ◽  
Shang-Jing Pan ◽  
...  
Keyword(s):  
Standard Method ◽  
Method Performance ◽  
Performance Requirements ◽  
Β Carotene

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.

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