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.

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%

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.

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.

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 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.

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 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 Free and Total Carnitine and Choline in Infant Formulas and Adult Nutritional Products by UPLC/MS/MS: Single-Laboratory Validation, First Action 2014.04

2015 ◽  
Vol 98 (5) ◽  
pp. 1395-1406 ◽  
Author(s):  
Wei Jing ◽  
Joseph J Thompson ◽  
Wesley A Jacobs ◽  
Louis M Salvati
Keyword(s):  
Microwave Digestion ◽  
Method Performance ◽  
Internal Validation ◽  
Expert Review ◽  
Performance Requirements ◽  
Expert Review Panel ◽  
Total Carnitine ◽  
Single Laboratory ◽  
Subsequent Neutralization

Abstract A single-laboratory validation (SLV) has been performed for a method that simultaneously determines choline and carnitine in nutritional products by ultra performance LC (UPLC)/MS/MS. All 11 matrixes from the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) were tested. Depending on the sample preparation, either the added (free, with a water dilution and filtering) or total (after microwave digestion at 120°C in nitric acid and subsequent neutralization with ammonia) species can be detected. For nonmilk containing products, the total carnitine is almost always equal to the free carnitine. A substantial difference was noted between free and total choline in all products. All Standard Method Performance Requirements for carnitine and choline have been met. This report summarizes the material sent to the AOAC Expert Review Panel for SPIFAN nutrient methods for the review of this method, as well as some additional data from an internal validation. The method was granted AOAC First Action status for carnitine in 2014 (2014.04), but the choline data are also being presented. A comparison of choline results to those from other AOAC methods is given.

Determination of total proteinogenic amino acids and taurine by pre-column derivatisation and UHPLC: Single Laboratory Validation, First Action 2019.09

2020 ◽  
Author(s):  
George Joseph ◽  
Asha Varughese ◽  
Ann Daniel
Keyword(s):  
Amino Acids ◽  
Amino Acid ◽  
Infant Formula ◽  
Retention Time ◽  
Sulfonic Acid ◽  
Internal Standard ◽  
The Other ◽  
Method Performance ◽  
Single Laboratory

Abstract Background A method has been developed and validated for selective, accurate and precise determination of total proteinogenic amino acids and taurine from Infant Formula and Adult/Pediatric Nutritional Formulas (powders, ready-to-feed liquids, and liquid concentrates). The method was reviewed by the AOAC INTERNATIONAL SPIFAN Expert Review Panel (ERP) during the 133rd AOAC Annual Meeting & Expo on September 7, 2019 in Denver, CO, USA and was recommended to First Action Official MethodsSM status. Objective The method involves protein hydrolysis to amino acids, a simple pre-column derivatisation of amino acids and separation of derivatised amino acids by UHPLC. The quantification of amino acids is performed by multi-point calibration using norvaline as the internal standard. The analytical method is capable of quantitative determination for 22 proteinogenic amino acids, but cannot be used to quantitate tryptophan, which is destroyed during the acid hydrolysis step. Asparagine is determined as aspartic acid and glutamine as glutamic acid. The cystine and cysteine are converted to S-2-carboxyethylthiocysteine (CYSx) and the derivative is separated from the other amino acids. Citrulline which is present in some matrices and it is separated from other amino acids is not included in the method performance evaluation in the single laboratory validation (SLV). Method The proposed method met all the performance requirement limits set in standard method performance requirements (SMPR) 2014.013 for total proteinogenic amino acids and taurine. The correlation coefficient of multi-point calibration was not less than 0.999 for any amino acids at any point in the SLV study confirming the validity of linear dynanic range (LDR) and linearity of the method. The individual amino acids in the chromatogram were identified by absolute retention time and relative retention time (RRT) with respect to the internal standard norvaline. There were no significant (S/N Ratio <10) interferences from the reagents or by-products of derivatisation and targeted matrices. The method demonstrated high selectivity. Result Accuracy of the method was validated using standard reference materials (NIST SRM 1869 and 1849a) and spike recovery studies. The amino acid results in the SRMs were within the ranges of Reference Mass Fraction Values. The accuracy of the method was corroboratively validated by spike recovery studies. The average spike recovery range between 93 to 107% ensure the accuracy of the method for amino acids and compliance to the AOAC SMPR 2014.013. Conclusions Precision data of the method demonstrate that it meets the stakeholder requirements as per the SMPR. The mean RSDr for all the amino acids for 17 matrices selected for the SLV were not more than 4%. The method is very sensitive and the LOQ can go down to approximately ten times lower than the SMPR requirements. The sensitivity of method is a direct reflection of its signal to noise ratio which ensures guaranteed method performance at the lower levels of amino acids in these matrices. Highlights Taurine (aminoethane sulfonic acid) unlike the other amino acids is a beta-sulfonic amino acid that is not used in protein synthesis but is found as a free amino acid in tissues. The acidic functional group (-COOH) in common amino acid is replaced with a sulfonic acid (-SO3H) group in Taurine. The method offers baseline separation of citrulline which is an alpha amino acid generally present in Infant Formula and Adult/Pediatric Nutritional products. The separation of citrulline eliminates the risk of interference of this compound with other amino acids. The method can also separate and quantitate hydroxyproline, an important component of collagen that is often used to quantitate collagen. The method is simple and does not include any proprietary chemicals or instruments and can be performed on any basic reverse phase UHPLC system with UV detection.

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