AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Tuesday

high-resolution quadrupole-time-of-flight mass spectrometer (Q-TOFMS) was employed as a secondary detector (connected in series to the LC-DAD instrument) to provide high confidence identification of target analytes. The obtained results demonstrate excellent performance of the method in quantitative analysis of important cannabinoids in dried plants, concentrates, and oils. Presenter: Katerina Mastovska, Eurofins Food Integrity & Innovation, Madison, WI, USA, Email: KaterinaMastovska@eurofinsUS.com P-T-032 John Schmitz , Katerina Mastovska , Eurofins Food Integrity & Innovation, Madison, WI, USA; Lukas Vaclavik , Eurofins Food Integrity & Innovation, Harrogate, United Kingdom Determination of Hemp Specific Terpenes in Hemp- Based Matrices Using Headspace GC-MS Terpenes contribute significantly to the overall aroma and flavor of hemp-based products. The combination and ratios of the terpenes are important to track in order to provide consum- ers with a profile of the expected aroma. In addition, batch to batch tracking allows for the mixing of different raw materials in order to create new aromas or maintain an aroma profile across multiple batches or raw material sources. A headspace gas chromatographic-mass spectrometric (GC-MS) method for more than forty different terpenes has been developed. Eighteen hemp-specific terpenes were evaluated for accuracy and precision in various hemp-based matrices. About twen- ty-five additional terpenes were included in the screen in order to expand the scope of the method in the future, possibly to other raw material types or essential oils. A novel interpretation of the full evaporation technique (FET) was evaluated in order to accurately quantify matrices that were oil-based and those that were powders. Chromatography and validation data statistics generated from various matrices at several spiking levels will be presented. Presenter: Katerina Mastovska, Eurofins Food Integrity & Innovation, Madison, WI, USA, Email: KaterinaMastovska@eurofinsUS.com P-T-033 John Schmitz , Matthew Eckert , Katerina Mastovska , Eurofins Food Integrity & Innovation, Madison, WI, USA; Lukas Vaclavik , Eurofins Food Integrity & Innovation, Harrogate, United Kingdom Determination of Residual Solvents in Hemp-Based Matrices Using Headspace GC-MS The advent and subsequent proliferation of novel hemp-based consumer products in the last 5-10 years has introduced an abundance of new products to the market. The manufacturers of these products want to use the best extraction method to isolate the desired components from the hemp stalk, seeds, leaves or other parts of the plant. Typical extraction methods use solvents or gases. Residual solvents and gases should be monitored in the raw materials generated or final products produced, in order to evaluate potential contamination of the product. A list of approximately thirty gases and solvents were compiled and evaluated for their performance using a USP <467>-based methodology. Several hemp-based products were spiked with

mixes of solvents and gases at low and higher levels in order to establish accuracy and precision of the method. The matrices included ground hemp, ground hemp seeds, hemp oil, CBD (cannabidiol)-infused gummies, and CBD isolate. Additional work was performed to include the many isomers of hexane, heptane, and the common components of petroleum ether. Validation data statistics generated from various matrices at several spiking levels will be presented. Presenter: Katerina Mastovska, Eurofins Food Integrity & Innovation, Madison, WI, USA, Email: KaterinaMastovska@eurofinsUS.com P-T-034 Philip Wylie , Jessica Westland , Agilent Technologies, Inc., Wilmington, DE, USA Astoundingly High Pesticide Residue Levels on Confiscated Cannabis A high-resolution, accurate mass GC/Q-TOF instrument was used to screen confiscated cannabis samples for more than 1000 pesticides and environmental contaminants. Each sample of ground dried cannabis flower was extracted in acetonitrile and the extract was passed through an end capped C-18 SPE cartridge. Because cannabis extracts are so dirty, they were diluted 125:1 with solvent. The GC method used was retention- time-locked to a commercially available Personal Compound Database and Library (PCDL) that contains accurate mass spectra and locked retention times for 1020 compounds. To make data review easier the original PCDL was used to create a subset PCDL containing about 250 pesticides that are most commonly found on food commodities in the US. Data files were reviewed using two different procedures for finding suspect compounds–Find by Fragments (FbF) and Unknowns Analysis (UA). Twenty-one samples of confiscated cannabis flower were analyzed and eleven were found to be contaminated with detectable pesticide residues. Thirteen different pesticides were tentatively identified using these procedures. Concentrations of some of these pesticides were determined by calibration with standards. Two cannabis samples had pesticide levels that were estimated to be about 10 times greater than the highest EPA tolerance set for food and about 4000 times greater than the Canadian MRLs for dried cannabis. Presenter: Philip Wylie, Agilent Technologies, Inc., Wilmington, DE, USA, Email: phil_wylie@agilent.com P-T-035 Kristie Adams , Steelyard Analytics, Inc., Gaithersburg, MD, USA; Jakob Waldthausen , Elina Hafer , Andreas Formes , Katharina Kraus , Bernd Diehl , Spectral Service AG, Cologne, Germany Method Development and qNMR Analysis of Finished Products Containing Cannabidiol (CBD) The worldwide cannabis market is growing at an astounding rate. Europe is set to become the largest market in the world for legal cannabis—potentially worth over €123 billion by 2028. However, the cannabidiol (CBD) market is also expe- riencing a large amount of growth, which, in the US, is due in part to recently relaxed regulations surrounding the growth of industrial hemp. Explosive growth in the cannabis product

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