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 Determination of Curcuminoids in Turmeric Raw Materials and Dietary Supplements by HPLC: Single-Laboratory Validation, First Action 2016.16

2018 ◽  
Vol 101 (1) ◽  
pp. 203-207 ◽  
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown
Keyword(s):  
Dietary Supplements ◽  
Standard Method ◽  
Raw Materials ◽  
Review Panel ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract The AOAC Expert Review Panel (ERP) approved a method for the quantitation of curcuminoids for consideration for First Action Official MethodSM status. The previously published method summarized a single-laboratory validation of three individual curcuminoinds—curcumin, demethoxycurcumin, and bis-demethoxycurcumin—in raw materials and finished products. Method performance was compared with AOAC Standard Method Performance Requirement 2016.003. With repeatability precision ranging from 0.3 to 5.5% and recoveries from 96.6 to 103.3% in the different product matrixes, the ERP adopted the method 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 Alkaloids in Mitragyna speciosa (Kratom) Raw Materials and Dietary Supplements by HPLC-UV: Single-Laboratory Validation, First Action 2017.14

2018 ◽  
Vol 101 (4) ◽  
pp. 964-965
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown
Keyword(s):  
Standard Method ◽  
Raw Materials ◽  
Review Panel ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Mitragyna Speciosa ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract The AOAC Expert Review Panel (ERP) approved a method for the quantitation of alkaloids in Mitragyna speciosa for consideration as First Action Official MethodSM status. The previously published method summarized a single-laboratory validation of two alkaloids, mitragynine and 7-hydroxymitragynine, in raw materials and finished products. The methods performance was compared with the AOAC Standard Method Performance Requirement 2015.008. With repeatability precision (RSDr) ranging from 0.51 to 0.95% and recoveries from 93.6 to 98.9% in the different product matrices, the ERP adopted the method and provided recommendations for achieving Final 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 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.

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.

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 Single Laboratory Validation of a Method for Determination of Glucosamine in RawMaterials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization

2004 ◽  
Vol 87 (5) ◽  
pp. 1083-1092 ◽  
Author(s):  
Joseph ZiQi Zhou ◽  
Ted Waszkuc ◽  
Felicia Mohammed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Raw Materials ◽  
Glucosamine Sulfate ◽  
Glucosamine Hydrochloride ◽  
Relative Standard ◽  
Single Laboratory

Abstract Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients >0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15, 100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations <0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study.

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 Biotin in Infant, Pediatric, and Adult Nutritionals by High-Performance Liquid Chromatography and Fluorescence Detection: Single-Laboratory Validation, First Action 2016.11

2017 ◽  
Vol 100 (1) ◽  
pp. 145-151 ◽  
Author(s):  
Qi Lin ◽  
Yi Ding ◽  
Fiona Poh ◽  
Chunyan Zhang ◽  
Shang-Jing Pan ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Metaphosphoric Acid ◽  
Expert Review ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A reversed-phase HPLC method with postcolumn protein conjugation and fluorescence detection for the quantitative determination of biotin in infant, pediatric, and adult nutritionals was developed and evaluated in a single-laboratory validation (SLV). Sample of appropriate size is mixed with 2% metaphosphoric acid to precipitate out the protein. The filtrate is injected onto a C18 HPLC column in which biotin and riboflavin are separated with an appropriate mobile phase. The biotin, after eluting from the column, binds with the streptavidin fluorescein to become a fluorescent conjugate. The conjugate is then detected by fluorescence at λex = 495 nm and λem = 518 nm. A column switch is used in the method as an option to shorten the run time from 30 to 15 min, by eluting out riboflavin at a higher flow rate. In this SLV, a total of 19 AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals matrixes representing a range of infant,pediatric, and adult formulas were evaluated for their biotin content. The analytical range was 1.66–142 μg/100 g reconstituted final product. The repeatability and intermediate precision ranged from 0.5 to 3.0% RSDr and from 1.3 to 4.5% RSDiR, respectively. Recovery from spiked matrixes varied from 95 to 111%, and accuracy of quantification using Standard Reference Material 1849a ranged from 99 to 105%. The LOQ in reconstituted product was estimated to be 0.8 μg/100 g. The method was approved by the Expert Review Panel as First Action at the 2016 AOAC INTERNATIONAL Mid-Year Meeting.

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