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 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 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 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 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.

scholarly journals Determination of Sugars in Beet and Cane Final Molasses by Ion Chromatography: Collaborative Study

1997 ◽  
Vol 80 (3) ◽  
pp. 603-610
Author(s):  
Kevin Schäffler ◽  
C M J Day-Lewis ◽  
Margaret Clarke ◽  
Jill Jekot ◽  
E Rearick ◽  
...  
Keyword(s):  
Ion Chromatography ◽  
High Performance ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Amperometric Detection ◽  
Pulsed Amperometric Detection ◽  
Cane Molasses ◽  
Beet Molasses ◽  
Repeatability And Reproducibility

Abstract A collaborative study of an ion chromatographic tech’ nique of high-performance anion-exchange with pulsed amperometric detection has been completed. The procedure was used to determine sucrose, glucose, and fructose in 8 cane molasses samples and sucrose in 5 beet molasses samples. Eleven laboratories took part in the study. Repeatability and reproducibility values for sucrose, glucose, and fructose were excellent for both types of samples. All criteria for accepting the method for sugars in both beet and cane molasses were met. The ion chromatographic method for determination of sugars in beet and cane final molasses has been adopted first action by AOAC INTERNATIONAL.

Determination of Lactose in Lactose-Free and Low-Lactose Milk, Milk Products, and Products Containing Dairy Ingredients by the LactoSens®R Amperometry Method: First Action 2020.01

2020 ◽  
Vol 103 (6) ◽  
pp. 1534-1546
Author(s):  
Elisabeth Halbmayr-Jech ◽  
Roman Kittl ◽  
Patrick Weinmann ◽  
Christopher Schulz ◽  
Anna Kowalik ◽  
...  
Keyword(s):  
Infant Formula ◽  
Dairy Products ◽  
Amperometric Detection ◽  
Exchange Chromatography ◽  
Method Performance ◽  
Milk Products ◽  
Performance Requirements ◽  
Dairy Ingredients ◽  
Milk And Dairy Products

Abstract Background The AOAC Stakeholder Panel on Strategic Food Analytical Methods approved Standard Method Performance Requirements (SMPR®) 2018.009 for lactose in low-lactose or lactose-free milk, milk products, and products containing dairy ingredients. The LactoSens®R Method is a biosensor assay kit developed for the determination of lactose in a variety of lactose-free or low-lactose milk, dairy, and infant formula products produced with yeast-neutral lactases. Objective In response to a call for methods, the LactoSensR method was validated in a single laboratory study with comparison to SMPR 2018.009. Method The LactoSensR method was evaluated for calibration, interference, repeatability, recovery, and robustness. In a method comparison study samples naturally containing low levels of lactose were evaluated using LactoSensR and an accredited high-performance anion-exchange chromatography with pulsed amperometric detection. Results Calibration with lactose standard solutions was shown to be linear and the method was shown to be free of interference from a variety of sugars, vitamins, alcohols, flavorings, and other compounds. Matrix studies, including 85 spiked materials, 55 products naturally containing lactose, and 13 reference materials, resulted in RSDr of 0–10.5% at 8–100 mg lactose/100 g and 0.2–5.4% at >100 mg lactose/100 g for milk and dairy products and 1.0–6.8% for infant formula, in compliance with SMPR 2018.009 with few exceptions. Recovery was 85.0–110.3% at 8–100 mg lactose/100 g and 85.6–109.7% at >100 mg lactose/100 g for milk and dairy products and 91.1–97.0% for infant formula, also meeting the performance requirements with few exceptions. The method was shown to be robust to changes in ambient temperature, sample temperature, and sample volume. Conclusions The LactoSensR method compares favorably with the requirements of SMPR 2018.009 and should be adopted as a First Action AOAC Official MethodSM. Highlights The LactoSensR method is a fast, easy-to-use method that meets the requirements of SMPR 2018.009.

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 Total, Soluble, and Insoluble Dietary Fiber in Foods—Enzymatic-Gravimetric Method, MES-TRIS Buffer: Collaborative Study

1992 ◽  
Vol 75 (3) ◽  
pp. 395-416 ◽  
Author(s):  
Sungsoo C Lee ◽  
Leon Prosky ◽  
Jonathan W De Vries
Keyword(s):  
Dietary Fiber ◽  
Collaborative Study ◽  
Gravimetric Method ◽  
Tris Buffer ◽  
Total Dietary Fiber ◽  
Method Performance ◽  
Insoluble Dietary Fiber ◽  
Heat Stable ◽  
Assay Precision

Abstract A joint AOAC/AACC (American Association of Cereal Chemists) collaborative study of methods for the determination of soluble, insoluble, and total dietary fiber (SDF, IDF, and TDF) was conducted with 11 participating laboratories. The assay Is based on a modification of the AOAC TDF method 985.29 and the SDF/IDF method collaboratively studied recently by AOAC. The principles of the method are the same as those for the AOAC dietary fiber methods 985.29 and 991.42, Including the use of the same 3 enzymes (heat-stable α-amylase, protease, and amyloglucosldase) and similar enzyme Incubation conditions. In the modification, minor changes have been made to reduce analysis time and to Improve assay precision: (1) MES-TRIS buffer replaces phosphate buffer; (2) one pH adjustment step Is eliminated; and (3) total volumes of reaction mixture and filtration are reduced. Eleven collaborators were sent 20 analytical samples (4 cereal and grain products, 3 fruits, and 3 vegetables) for duplicate blind analysis. The SDF, IDF, and TDF content of the foods tested ranged from 0.53 to 7.17, 0.59 to 60.53, and 1.12 to 67.56 g/100 g, respectively. The respective average RSDR values for SDF, IDF, and TDF determinations by direct measurements were 13.1, 5.2, and 4.5%. The TDF values calculated by summing SDF and IDF were in excellent agreement with the TDF values measured independently. The modification did not alter the method performance with regard to mean dietary fiber values, yet It generated lower assay variability compared with the unmodified methods. The method for SDF, IDF, and TDF (by summing SDF and IDF) has been adopted first action by AOAC International.

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