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.

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 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 Withanolides in Withania somnifera by Liquid Chromatography: Single-Laboratory Validation, First Action 2015.17

2016 ◽  
Vol 99 (6) ◽  
pp. 1444-1458 ◽  
Author(s):  
Rojison Koshy ◽  
Mayachari Shivanand Anand ◽  
Balasubramanian Murali ◽  
Sharon L Brunelle
Keyword(s):  
Withania Somnifera ◽  
Raw Material ◽  
Performance Criteria ◽  
Method Performance ◽  
Performance Requirement ◽  
Expert Review ◽  
Withanolide A ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract An LC method was developed and validated in 2007 for analyzing Withania somnifera raw material (root) and dried extracts for withanolide content, including withanoside IV, withanoside V, withaferin A, 12-deoxywithastromonolide, withanolide A, and withanolide B. The method involved the extraction of the analytes with methanol, their subsequent filtration, and then analysis on a C18 column with an acetonitrile gradient and UV detection. Single-laboratory validation yielded linearity generally in the range of 20 to 200 μg/mL for each analyte, with a repeatability precision of RSD < 3% in most cases, and recovery in the range of 90 to 105%. These results compare well with the performance criteria recently detailed in AOAC Standard Method Performance Requirement 2015.007. The method was shown to be rugged with respect to different analysts, equipment, and days of analysis, and the sample solution was shown to be stable for 24 h at room temperature after extraction. The method was reviewed by the AOAC Expert Review Panel on Dietary Supplements (Set 2 Ingredients) and approved for First Action Official MethodSM status.

Determination and Confirmation of Parent and Total Ractopamine in Bovine, Swine, and Turkey Tissues by Liquid Chromatography with Tandem Mass Spectrometry: First Action 2011.23

2012 ◽  
Vol 95 (5) ◽  
pp. 1235-1255 ◽  
Author(s):  
Thomas J Burnett ◽  
John M Rodewald ◽  
Sharon L Brunelle ◽  
Mark Neeley ◽  
Michael Wallace ◽  
...  
Keyword(s):  
Internal Standard ◽  
Veterinary Drug ◽  
Review Panel ◽  
Validation Data ◽  
Expert Review ◽  
Maximum Residue Limits ◽  
Initial Extract ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A candidate method selected by the AOAC Expert Review Panel (ERP) for Ractopamine for determination and confirmation of parent and total ractopamine by LC/MS/MS was validated in a single laboratory for bovine, swine, and turkey tissues. The candidate method utilizes methanol extraction of the tissues, followed by an optional enzymatic hydrolysis for determination of total (parent plus conjugate) ractopamine. A mixed-mode cation exchange SPE cartridge is used to purify the initial extract before LC/MS/MS. Matrix-matched standards and a ractopamine-d6 internal standard are used for quantification of parent and total ractopamine in unknown samples. Validation data demonstrated that mean intertrial recoveries for ractopamine across all concentrations tested ranged from 79.7 to 102.2% for parent ractopamine and from 79.0 to 100.0% when a hydrolysis step was included. Intertrial repeatability precision ranged from 2.44 to 11.1% for parent ractopamine and 4.97 to 15.0% with hydrolysis. Estimated LOD values were below 0.1 ng/g and LOQ values were validated at 0.25x the maximum residue limits. The data satisfy the requirements of the AOAC Stakeholder Panel for Veterinary Drug Residue Methods for single laboratory validation studies. The method was awarded Official Methods of AnalysisSM First Action 2011.23 by the AOAC ERP on Veterinary Drug Residues.

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 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%

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.

Determination of Ractopamine in Swine, Bovine, and Turkey Tissues by HPLC with Fluorescence Detection: First Action 2011.22

2012 ◽  
Vol 95 (4) ◽  
pp. 945-958 ◽  
Author(s):  
Thomas J Burnett ◽  
John M Rodewald ◽  
John Moran ◽  
Michael P Turberg ◽  
Sharon L Brunelle ◽  
...  
Keyword(s):  
Bovine Liver ◽  
Veterinary Drug ◽  
Review Panel ◽  
Expert Review ◽  
Veterinary Drug Residue ◽  
Maximum Residue Limits ◽  
Swine Liver ◽  
Expert Review Panel ◽  
Single Laboratory

Abstract A candidate LC method proposed by the Expert Review Panel (ERP) for ractopamine was evaluated in a single-laboratory validation (SLV) study. The matrixes examined included bovine liver, kidney, muscle, and fat; swine liver, kidney, muscle, and fat; and turkey liver and muscle. Solution standards were shown to provide a linear response with an unweighted regression. The method demonstrated acceptable precision (HorRatr values 0.25 to 1.38) and recovery (75.4 to 88.8%) in all fortified matrixes. Method precision was verified with incurred residue tissues (bovine liver, kidney, and muscle; swine liver, kidney, and muscle; and turkey liver and muscle), which yielded RSDr values below 16% for all tissues and below 7% for most tissues. Estimated LOQ values ranged from 1.8 to 20.7 ng/g and support the utility of the method in the range of the maximum residue limits or tolerances for the various tissues. The data satisfy the requirements of the AOAC Stakeholder Panel on Veterinary Drug Residue for SLV studies, and the method was adopted Official Methods of AnalysisSM First Action 2011.22 by the AOAC ERP on Veterinary Drug Residues.

Evaluation Protocol for Review of Method Validation Data by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals Expert Review Panel

2015 ◽  
Vol 98 (1) ◽  
pp. 112-115 ◽  
Author(s):  
Brendon D Gill ◽  
Harvey E Indyk ◽  
Christopher J Blake ◽  
Erik J M Konings ◽  
Wesley A Jacobs ◽  
...  
Keyword(s):  
Dispute Resolution ◽  
Infant Formula ◽  
Standard Method ◽  
Review Panel ◽  
Validation Data ◽  
Method Performance ◽  
Expert Review ◽  
Evaluation Protocol ◽  
Validation Parameters ◽  
Expert Review Panel

Abstract Methods under consideration as part of the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals process are to be evaluated against a set of Standard Method Performance RequirementsSM(SMPRs) via peer review by an expert review panel (ERP). A validation protocol and a checklist have beendeveloped to assist the ERP to evaluate experimentaldata and to compare multiple candidate methods for each nutrient. Method performance against validation parameters mandated in the SMPRs as well as additional criteria are to be scored, with the method selected by the ERP proceeding to multilaboratory study prior to Final Action approval. These methods are intended to be used by the infant formula industry for the purposes of dispute resolution.

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