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

2013 ◽  
Vol 96 (4) ◽  
pp. 917-924 ◽  
Author(s):  
W Dennis Ulrey ◽  
Thomas J Burnett ◽  
Sharon L Brunelle ◽  
Kimberly R Lombardi ◽  
Mark R Coleman
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
Bovine Liver ◽  
The United States ◽  
Tandem Mass ◽  
Review Panel ◽  
Expert Review ◽  
Swine Liver ◽  
Expert Review Panel ◽  
Aoac Official

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.

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.

scholarly journals Dhb Microcystins Discovered in USA Using an Online Concentration LC–MS/MS Platform

Toxins ◽  
2019 ◽  
Vol 11 (11) ◽  
pp. 653 ◽  
Author(s):  
Johnna A. Birbeck ◽  
Nicholas J. Peraino ◽  
Grace M. O’Neill ◽  
Julia Coady ◽  
Judy A. Westrick
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
United States Of America ◽  
Algal Bloom ◽  
Harmful Algal Bloom ◽  
The United States ◽  
Tandem Mass ◽  
Chemical Derivatization ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Based on current structural and statistical calculations, thousands of microcystins (MCs) can exist; yet, to date, only 246 MCs were identified and only 12 commercial MC standards are available. Standard mass spectrometry workflows for known and unknown MCs need to be developed and validated for basic and applied harmful algal bloom research to advance. Our investigation focuses on samples taken in the spring of 2018 from an impoundment fed by Oser and Bischoff Reservoirs, Indiana, United States of America (USA). The dominant cyanobacterium found during sampling was Planktothrix agardhii. The goal of our study was to identify and quantify the MCs in the impoundment sample using chemical derivatization and mass spectrometry. Modifying these techniques to use online concentration liquid chromatography tandem mass spectrometry (LC–MS/MS), two untargeted MCs have been identified, [d-Asp3, Dhb7]-MC-LR and [Dhb7]-MC-YR. [Dhb7]-MC-YR is not yet reported in the literature to date, and this was the first reported incidence of Dhb MCs in the United States. Furthermore, it was discovered that the commercially available [d-Asp3]-MC-RR standard was [d-Asp3, Dhb7]-MC-RR. This study highlights a workflow utilizing online concentration LC–MS/MS, high-resolution MS (HRMS), and chemical derivatization to identify isobaric MCs.

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 ◽  
...  
Keyword(s):  
Data Sets ◽  
Acceptance Criteria ◽  
Review Panel ◽  
Expert Review ◽  
Expert Review Panel ◽  
Aoac Official

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.

scholarly journals Direct aqueous injection of the fluoroacetate anion in potable water for analysis by liquid chromatography tandem mass-spectrometry

2018 ◽  
Vol 10 (46) ◽  
pp. 5524-5531 ◽  
Author(s):  
Emily Parry ◽  
Stuart A. Willison
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Potable Water ◽  
The United States ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Direct Aqueous Injection

Sodium fluoroacetate or Compound 1080 is a rodenticide registered in the United States for use in livestock protection collars.

scholarly journals Non-targeted Screening of Commercial CBD Products in the United States Reveals Common Contamination and Adulteration

2020 ◽  
Author(s):  
Ben Orsburn
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
High Resolution ◽  
The United States ◽  
Mass Spectrometry Data ◽  
Accurate Mass ◽  
Targeted Screening ◽  
Accurate Mass Spectrometry ◽  
High Concentrations ◽  
High Resolution Accurate Mass

AbstractThe production of hemp and products derived from these plants that contain zero to trace amounts of the psychoactive cannabinoid tetrahydrocannabidiol (THC) is a rapidly growing new market in the United States. The most common products today contain relatively high concentrations of the compound cannabidiol (CBD). Recent studies have investigated commercial CBD products using targeted assays and have found varying degrees of misrepresentation and contamination of these products. To expand on previous studies, we demonstrate the application of non-targeted screening by high resolution accurate mass spectrometry to more comprehensively identify potential adulterants and contaminants. We find evidence to support previous conclusions that CBD products are commonly misrepresented in terms of cannabinoid concentrations present. Specifically, we observe a wide variation in relative THC concentrations across the product tested, with some products containing 10-fold more relative signal than others. In addition, we find that several products appear to be purposely adulterated with over the counter drugs such as caffeine and melatonin. We also observe multiple small molecule contaminants that are typically linked to improper production or packaging methods in food or pharmaceutical production. Finally, we present high resolution accurate mass spectrometry data and tandem MS/MS fragments supporting the presence of trace amounts of fluorofentanyl in a single mail order CBD product. We conclude that the CBD industry would benefit from more robust testing regulations and that the cannabis testing industry, in general, would benefit from the use of non-targeted screening technologies.

scholarly journals Simultaneous Determination of Zilpaterol and Other Beta Agonists in Calf Eye by Gas Chromatography/Tandem Mass Spectrometry

2003 ◽  
Vol 86 (1) ◽  
pp. 8-14 ◽  
Author(s):  
Beatrice Bocca ◽  
Maurizio Fiori ◽  
Claudia Cartoni ◽  
Gianfranco Brambilla
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Growth Promotion ◽  
The United States ◽  
Meat Production ◽  
Tandem Mass ◽  
Retinal Tissue ◽  
Chromatography Tandem Mass Spectrometry

Abstract Adrenergic drugs for growth promotion have been outlawed in European meat production; however, molecules such as Ractopamine and Zilpaterol are licensed for feeding swine and cattle in the United States, Mexico, and South Africa. Analysis of bovine retinal extracts has recently shown considerable extension in the detection period following withdrawal. Previous studies demonstrated that residual concentrations of Clenbuterol and related substances in retinal tissue were >100 ng/g at day 50 of withdrawal. A method was developed to identify and simultaneously quantify Clenbuterol-like substances with anilinic moieties and drugs with phenolic and catecholic moieties, such as Ractopamine and Zilpaterol, in retinal tissue. The method was validated according to SANCO/1805/2000. After extraction in 0.1N HCl, samples were cleaned up on C18 non-endcapped solid-phase extraction columns and analyzed as trimethylchlorosilane derivatives by gas chromatography/tandem mass spectrometry, electron impact mode. At concentrations of agonists between 62.5 and 250.0 ng/g in bovine retina, mean recoveries ranged from 85.3 to 94.8%, repeatability was <9.6%, and within-laboratory reproducibility was <10.5%. The decision limits (CCα) were within the range of 66.3–70.4 ng/g, and the detection capability (CCβ) varied from 73.9 to 79.8 ng/g. Results are discussed in terms of a multiresidue approach to improve reliability of the monitoring strategy.

scholarly journals Radiology Department Preparedness for COVID-19: Radiology Scientific Expert Review Panel

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 ◽  
...  
Keyword(s):  
Radiology Department ◽  
Review Panel ◽  
Expert Review ◽  
Expert Review Panel

Emerging Synthetic Cannabinoids: Development and Validation of a Novel Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry Assay for Real-Time Detection

2019 ◽  
Vol 44 (3) ◽  
pp. 207-217 ◽  
Author(s):  
Alex J Krotulski ◽  
Amanda L A Mohr ◽  
Barry K Logan
Keyword(s):  
United States ◽  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Real Time ◽  
Synthetic Cannabinoids ◽  
Time Of Flight ◽  
Forensic Toxicology ◽  
The United States ◽  
Synthetic Cannabinoid ◽  
Flight Mass Spectrometry

Abstract Synthetic cannabinoids pose significant threats to public health and safety, as their implications in overdose and adverse events continue to arise in United States and around the world. Synthetic cannabinoids have seen several generations of chemically diverse structural elements, impacting potency and effects. These factors create new analytical challenges for forensic laboratories. This report describes an efficient liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) assay for the identification of synthetic cannabinoid parent compounds and metabolites, including real-time identification of emergent compounds, using a SCIEX TripleTOF® 5600+ with non-targeted SWATH® acquisition. Method validation evaluated precision/accuracy, limits of detection, interferences, processed sample stability and carryover, for which 19 parent compounds and 19 metabolites were tested. To demonstrate feasibility, de-identified blood sample extracts were acquired from a large forensic toxicology laboratory and analyzed using the validated LC-QTOF-MS assay. In mid-2018, 200 blood extracts were analyzed, demonstrating a 19% positivity rate with > 94% agreement rate with original testing. In addition, three newly discovered synthetic cannabinoids were identified, including 5F-MDMB-PICA, 4-cyano CUMYL-BUTINACA and 5F-EDMB-PINACA. These synthetic cannabinoids were previously unreported in forensic toxicology casework in the United States. 5F-MDMB-PICA has become the most prevalent synthetic cannabinoid in United States, as of early 2019. These results demonstrate the effectiveness of this assay and workflow in the identification and characterization of synthetic cannabinoids, as well as the usefulness of sample-mining using non-targeted mass acquisition by LC-QTOF-MS for the discovery of NPS. High resolution mass spectrometry should be considered when developing new or novel assays for synthetic cannabinoids.

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