Analysis of Flutianil\nand OC56635 Residues in Hemp\nCannabis Matrices by LC-MS/MS

In this paper, we present analytical\nmethodologies for\nthe determination\nof the thiazolidine fungicide flutianil (trade name GATTEN) and its\nprimary metabolite OC56635 in hemp cannabis matrices. A total of nine\ncrop matrices were tested: whole seed, fiber, flower buds, hemp hearts,\nhemp seed oil, hemp meal, hemp flour, ethanol extracted CBD resin\n(CBD-E), and supercritical CO<sub>2</sub> extracted CBD resin (CBD-C).\nProcessing of the CBD-E and CBD-C crop fractions was carried out in-house\nusing methods detailed herein. Field sample analysis utilized sequential\nextractions, stacked solid phase extraction (SPE) column cleanups,\nand evaporation to prepare the samples for LC-MS/MS quantitation.\nMethod validations for each fraction were carried out using untreated\nhemp matrices over a minimum of three levels, with lowest levels of\nmethod validation (LLMV) of 0.010 μg/g for all fractions except\nthe CBD resins, for which LLMV was 0.020 μg/g. Flutianil-treated\nsamples from nine field sites were collected from several crop production\nregions and analyzed to determine the distribution of incurred flutianil\nand OC56635 residues within the different hemp matrices. This data\nwas generated in support of nationwide registration with the United\nStates Environmental Protection Agency (USEPA).

Publication Details

Journal
Figshare
Published
2024-08-14
DOI
https://doi.org/10.1021/acs.jafc.4c05103.s001
Primary Topic
Ion Channels and Receptors
Type
article
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article

Analysis of Flutianil\nand OC56635 Residues in Hemp\nCannabis Matrices by LC-MS/MS

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Ion Channels and Receptors
article

Analysis of Flutianil\nand OC56635 Residues in Hemp\nCannabis Matrices by LC-MS/MS

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Abstract

In this paper, we present analytical\nmethodologies for\nthe determination\nof the thiazolidine fungicide flutianil (trade name GATTEN) and its\nprimary metabolite OC56635 in hemp cannabis matrices. A total of nine\ncrop matrices were tested: whole seed, fiber, flower buds, hemp hearts,\nhemp seed oil, hemp meal, hemp flour, ethanol extracted CBD resin\n(CBD-E), and supercritical CO<sub>2</sub> extracted CBD resin (CBD-C).\nProcessing of the CBD-E and CBD-C crop fractions was carried out in-house\nusing methods detailed herein. Field sample analysis utilized sequential\nextractions, stacked solid phase extraction (SPE) column cleanups,\nand evaporation to prepare the samples for LC-MS/MS quantitation.\nMethod validations for each fraction were carried out using untreated\nhemp matrices over a minimum of three levels, with lowest levels of\nmethod validation (LLMV) of 0.010 μg/g for all fractions except\nthe CBD resins, for which LLMV was 0.020 μg/g. Flutianil-treated\nsamples from nine field sites were collected from several crop production\nregions and analyzed to determine the distribution of incurred flutianil\nand OC56635 residues within the different hemp matrices. This data\nwas generated in support of nationwide registration with the United\nStates Environmental Protection Agency (USEPA).

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