Elizabeth Mudge

National Research Council Canada

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Paula N. Brown

Sheffield Teaching Hospitals NHS Foundation Trust

Scott G Coates

Hertfordshire Community NHS Trust

Aniko M Sólyom

Analytical Services

Catherine A. Rimmer

National Institute of Standards and Technology

Melissa Phillips

National Institute of Standards and Technology

Garrett Zielinski

Covance (United States)

Brian T Schaneberg

Starbucks (United States)

Joseph M. Betz

Office of Dietary Supplements

Darryl Sullivan

Eurofins (United States)

John Szpylka

Institut Mérieux (France)

Cooperative Institutions

National Institute of Standards and Technology

Covance (United States)

University of Waikato

Cawthron Institute

British Columbia Institute of Technology

National Research Council Canada

Institute for Marine Biosciences

National Institute of Standards

United States Pharmacopeial Convention

Norwegian Veterinary Institute

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AOAC SMPR® 2016.004

Journal of AOAC International (2016)

Richard A. Myers Joseph M. Betz Maria Bøjstrup Neal E. Craft Heather Figore

10.5740/jaoacint.smpr2016.004

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Citations (1)

AOAC SMPR® 2017.001:Standard Method Performance Requirements (SMPRs) for Quantitation of Cannabinoids in Cannabis Concentrates

Journal of AOAC International (2017)

Susan Audino Mark Angerhofer Patricia Atkins Roger M Brauninger Paula N. Brown

Synthetic cannabinoids

Dronabinol

10.5740/jaoacint.smpr2017_001

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Citations (10)

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

Journal of AOAC International (2017)

Elizabeth Mudge Paula N. Brown

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.

Repeatability

10.5740/jaoacint.17-0111

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Citations (11)

Quantification of pyrrolizidine alkaloids in North American plants and honey by LC-MS: single laboratory validation

Food Additives & Contaminants Part A (2015)

Elizabeth Mudge A. Maxwell P. Jones Paula N. Brown

Pyrrolizidine alkaloids (PAs) are a class of naturally occurring compounds produced by many flowering plants around the World. Their presence as contaminants in food systems has become a significant concern in recent years. For example, PAs are often found as contaminants in honey through pollen transfer. A validated method was developed for the quantification of four pyrrolizidine alkaloids and one pyrrolizidine alkaloid N-oxide in plants and honey grown and produced in British Columbia. The method was optimised for extraction efficiency from the plant materials and then subjected to a single-laboratory validation to assess repeatability, accuracy, selectivity, LOD, LOQ and method linearity. The PA content in plants ranged from1.0 to 307.8 µg/g with repeatability precision between 3.8 and 20.8% RSD. HorRat values were within acceptable limits and ranged from 0.62 to 1.63 for plant material and 0.56–1.82 for honey samples. Method accuracy was determined through spike studies with recoveries ranging from 84.6 to 108.2% from the raw material negative control and from 82.1–106.0 % for the pyrrolizidine alkaloids in corn syrup. Based on the findings in this single-laboratory validation, this method is suitable for the quantitation of lycopsamine, senecionine, senecionine N-oxide, heliosupine and echimidine in common comfrey (Symphytum officinale), tansy ragwort (Senecio jacobaea), blueweed (Echium vulgare) and hound's tongue (Cynoglossum officinale) and for PA quantitation in honey and found that PA contaminants were present at low levels in BC honey.

Repeatability

Pyrrolizidine alkaloid

10.1080/19440049.2015.1099743

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Citations (28)

In Vitro Metabolism of Azaspiracids 1–3 with a Hepatopancreatic Fraction from Blue Mussels (Mytilus edulis)

Journal of Agricultural and Food Chemistry (2021)

Morten Sandvik Christopher O. Miles Kjersti Liv Eriksen Løvberg Fedor Kryuchkov Elliott J. Wright

Azaspiracids (AZAs) are a group of biotoxins produced by the marine dinoflagellates Azadinium and Amphidoma spp. that can accumulate in shellfish and cause food poisoning in humans. Of the 60 AZAs identified, levels of AZA1, AZA2, and AZA3 are regulated in shellfish as a food safety measure based on occurrence and toxicity. Information about the metabolism of AZAs in shellfish is limited. Therefore, a fraction of blue mussel hepatopancreas was made to study the metabolism of AZA1–3 in vitro. A range of AZA metabolites were detected by liquid chromatography–high-resolution tandem mass spectrometry analysis, most notably the novel 22α-hydroxymethylAZAs AZA65 and AZA66, which were also detected in naturally contaminated mussels. These appear to be the first intermediates in the metabolic conversion of AZA1 and AZA2 to their corresponding 22α-carboxyAZAs (AZA17 and AZA19). α-Hydroxylation at C-23 was also a prominent metabolic pathway, producing AZA8, AZA12, and AZA5 as major metabolites of AZA1–3, respectively, and AZA67 and AZA68 as minor metabolites via double-hydroxylation of AZA1 and AZA2, but only low levels of 3β-hydroxylation were observed in this study. In vitro generation of algal toxin metabolites, such as AZA3, AZA5, AZA6, AZA8, AZA12, AZA17, AZA19, AZA65, and AZA66 that would otherwise have to be laboriously purified from shellfish, has the potential to be used for the production of standards for analytical and toxicological studies.

Blue mussel

Hepatopancreas

Marine toxin

Shellfish Poisoning

Hydroxylation

Metabolic pathway

10.1021/acs.jafc.1c03831

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Citations (8)

Curcuminoids in Turmeric Roots and Supplements: Method Optimization and Validation

Food Analytical Methods (2015)

Elizabeth Mudge Michael Chan Sylesh K. Venkataraman Paula N. Brown

Curcuma longa L. rhizomes are used extensively as a spice in food preparations and dietary supplements for their anti-inflammatory and antioxidant properties. An expert review panel (ERP) evaluated analytical methods for the quantitation of individual curcuminoids for the purpose of identifying a method for official method status. It was requested that several modifications be undertaken to improve method performance prior to subjecting the chosen method to a single-laboratory validation. Two separate Plackett-Burman factorial studies were used to identify factors that contributed to the chromatographic separation and extraction of curcuminoids. Significant factors were further optimized to produce the improved HPLC method for curcuminoid separation. This method was then subjected to a single-laboratory validation according to the AOAC International guidelines for linearity, detection limits, precision, and accuracy. The two most significant factors impacting the quantitation of curcuminoids were column temperature and extraction solvent, which were optimized to 55 °C and 100 % methanol, respectively. The validation was performed on 12 raw materials and finished products containing turmeric roots. The method precision was reported using HorRat values which were within recommended ranges of the AOAC guidelines. Overall accuracy of the method was accessed at three separate levels for each analyte and ranged from 99.3–100.9 %. The validated method is suitable for quantitation of individual curcuminoids in turmeric raw materials and finished products and is recommended for consideration as an official method by the AOAC International.

Curcuminoid

Fractional factorial design

Plackett–Burman design

10.1007/s12161-015-0326-0

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Citations (36)

AOAC SMPR® 2017.010:Standard Method Performance Requirements (SMPRs) for Identification of Aloe Vera in Dietary Supplements and Dietary Ingredients

Journal of AOAC International (2017)

Prashant Ingle Brad Barrett Joseph M. Betz Clyde Don Nour‐Eddine Es‐Safi

Aloe Vera

Identification

Dietary supplement

10.5740/jaoacint.smpr2017_010

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Citations (0)

AOAC SMPR^® 2017.011

Journal of AOAC International (2017)

Garrett Zielinski Gisele Atkinson Sneh Bhandari Paul Burns Danielle Citrolo

10.5740/jaoacint.smpr2017_011

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Citations (3)

Determination of Aloin A and Aloin B in Aloe vera Raw Materials and Finished Products by High-Performance Liquid Chromatography: Single-Laboratory Validation

Journal of AOAC International (2014)

Paula N. Brown Ronan Yu Chiow Hui Kuan Jamie Finley Elizabeth Mudge

A single-laboratory validation (SLV) was conducted on an HPLC method for the detection and quantification of aloin A and aloin B in Aloe vera raw materials and finished products. An extraction procedure using sonication with an acidified solvent was used for solid test materials while liquid test materials only required dilution, if necessary, prior to filtration and analysis. Separation was achieved using a fused core C18 column in 18 min under isocratic elution conditions allowing for a single analyte (aloin A) calibration curve to quantify both aloins. Adequate chromatographic resolution (Rs ≥1) was achieved for aloin A and aloin B. The calibration curves for aloin A exhibited coefficients of determination (r2) of ≥99.9% over the linear range of 0.3–50 μg/mL. The LOD values were 0.092 and 0.087 μg/mL, and LOQ 0.23 and 0.21 μg/mL for aloin A and aloin B, respectively. Repeatability studies were performed on nine test materials on each of 3 separate days, with five of the test materials determined to be above the LOQ having repeatability RSD (RSDr) values ranging from 0.61 to 6.30%. Method accuracy was determined through a spike recovery study on both liquid and solid matrixes at three different levels: low, medium, and high. For both aloins, the recovery in the liquid matrix ranged from 92.7 to 106.3% with an RSDr of 0.15 to 4.30%, while for the solid matrix, the recovery ranged from 84.4 to 108.9% with an RSDr of 0.23 to 3.84%. Based on the results of the SLV study, it is recommended that this method be evaluated for reproducibility through a collaborative study.

Repeatability

Aloe Vera

Matrix (chemical analysis)

10.5740/jaoacint.13-028

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Citations (16)

In Situ Rheo‐NMR Measurements of Solid Fat Content

Journal of the American Oil Chemists Society (2008)

Gianfranco Mazzanti Elizabeth Mudge Emmanuel Y. Anom

Abstract The properties of crystallized fats depend on their solid fat content (SFC) and their fractal structures. The SFC and the structures are dramatically affected during crystallization under shear flow. A mini‐Couette cell was developed to crystallize fat samples under shear. The cell was tested with blends of canola stearin (CS) in canola oil (CO) in a 20‐MHz NMR spectrometer. The blends were placed in the cell, melted at 80 °C, and then crystallized under different shear rates (58–460 s −1 ) at 40 °C inside the spectrometer for 4 h. Time averaged NMR free induction decay (FID) curves were captured at 20 s intervals. SFC values were calculated using parameters determined by a calibration procedure. The SFC values determined by the direct method with and without the shaft of the Couette device were reasonably close. Similar results were observed with and without shear in the Couette device. The FID curves did not show a significant difference either. Therefore this system is accurate for in‐situ time‐resolved determination of SFC under shear flow. Furthermore, a combination of the direct and the indirect methods was successfully used to estimate the temperature increase due to viscous heating. The system developed will help in understanding the effects of shear flow on SFC of nanostructured lipid multicomponent systems. This will permit the optimization of the manufacturing processes.

10.1007/s11746-008-1227-9

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Citations (25)