Determination and Confirmation of Narasin and Monensin in Chicken, Swine, and Bovine Tissues by LC/MS/MS: Final Action 2011.24

2013 ◽  
Vol 96 (4) ◽  
pp. 902-909 ◽  
Author(s):  
Kimberly R Lombardi ◽  
Thomas J Burnett ◽  
Sharon L Brunelle ◽  
W Dennis Ulrey ◽  
Mark R Coleman ◽  
...  

Abstract A multilaboratory study was conducted to validate the reproducibility of AOAC Official MethodSM 2011.24 for determination of narasin and monensin in chicken, swine, and bovine tissues. This study was intended to satisfy requirements for Final Action status through the AOAC Expert Review Panel process. Ten laboratories participated in the study, analyzing blind duplicates of five incurred residue materials for each analyte. After removal of invalid data sets, the method reproducibility (RSDR 12.8–60.6%, HorRat 0.45–1.47) was within AOAC acceptance criteria. The method was awarded Final Action status by the Official Methods Board on October 4, 2012.

2012 ◽  
Vol 95 (5) ◽  
pp. 1235-1255 ◽  
Author(s):  
Thomas J Burnett ◽  
John M Rodewald ◽  
Sharon L Brunelle ◽  
Mark Neeley ◽  
Michael Wallace ◽  
...  

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.


2018 ◽  
Vol 101 (4) ◽  
pp. 964-965
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown

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.


2018 ◽  
Vol 101 (1) ◽  
pp. 203-207 ◽  
Author(s):  
Elizabeth M Mudge ◽  
Paula N Brown

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.


2012 ◽  
Vol 95 (4) ◽  
pp. 945-958 ◽  
Author(s):  
Thomas J Burnett ◽  
John M Rodewald ◽  
John Moran ◽  
Michael P Turberg ◽  
Sharon L Brunelle ◽  
...  

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.


2012 ◽  
Vol 95 (2) ◽  
pp. 313-318 ◽  
Author(s):  
Karen Schimpf ◽  
Renee Spiegel ◽  
Linda Thompson ◽  
Dawn Dowell

Abstract During the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held on June 29, 2011, an Expert Review Panel (ERP) reviewed the method “Determination of Vitamin B12 in Infant Formula and Adult Nutritionals by HPLC.” Under the new pathway to Official MethodsSM, the ERP adopted the method as Official First Action. The method is applicable to the determination of vitamin B12 in infant formula and adult nutritionals. Data showed an average overall intermediate precision of 6.64% RSD, an estimated quantitation limit of 0.8 μg/kg, and a detection limit of 0.2 μg/kg in prepared samples. The standard range of the method is 2 to 200 μg/L, which corresponds to an analytical range of 0.8 to 500 μg/kg.


2013 ◽  
Vol 96 (4) ◽  
pp. 802-807 ◽  
Author(s):  
Karen Schimpf ◽  
Linda Thompson ◽  
Steve Baugh

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.


2013 ◽  
Vol 96 (4) ◽  
pp. 917-924 ◽  
Author(s):  
W Dennis Ulrey ◽  
Thomas J Burnett ◽  
Sharon L Brunelle ◽  
Kimberly R Lombardi ◽  
Mark R Coleman

Abstract A multilaboratory study of AOAC Official MethodSM 2011.23 was performed to satisfy requirements for Final Action status through the AOAC expert review panel process. The study included nine collaborating laboratories from the United States, Canada, Brazil, and The Netherlands. Five incurred residue materials (bovine muscle, bovine liver, swine muscle, swine liver, and turkey muscle) were analyzed by each laboratory as blind duplicates for parent and total ractopamine content. After removal of invalid data, the parent and total ractopamine methods demonstrated acceptable reproducibility (RSDR 11.4–42.4%, HorRatR 0.34–2.01) based on AOAC criteria. The method was awarded Final Action status by the Official Methods Board on October 4, 2012.


Radiology ◽  
2020 ◽  
Vol 296 (2) ◽  
pp. E106-E112 ◽  
Author(s):  
Mahmud Mossa-Basha ◽  
Carolyn C. Meltzer ◽  
Danny C. Kim ◽  
Michael J. Tuite ◽  
K. Pallav Kolli ◽  
...  

2016 ◽  
Vol 99 (1) ◽  
pp. 53-54
Author(s):  
Sharon L Brunelle

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.


2016 ◽  
Vol 99 (1) ◽  
pp. 242-251 ◽  
Author(s):  
Lauren M Fleury ◽  
Bryan G Scahill ◽  
Rilka Taskova

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.


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