In this paper, we present analytical
methodologies for
the determination
of the thiazolidine fungicide flutianil (trade name GATTEN) and its
primary metabolite OC56635 in hemp cannabis matrices. A total of nine
crop matrices were tested: whole seed, fiber, flower buds, hemp hearts,
hemp seed oil, hemp meal, hemp flour, ethanol extracted CBD resin
(CBD-E), and supercritical CO2 extracted CBD resin (CBD-C).
Processing of the CBD-E and CBD-C crop fractions was carried out in-house
using methods detailed herein. Field sample analysis utilized sequential
extractions, stacked solid phase extraction (SPE) column cleanups,
and evaporation to prepare the samples for LC-MS/MS quantitation.
Method validations for each fraction were carried out using untreated
hemp matrices over a minimum of three levels, with lowest levels of
method validation (LLMV) of 0.010 μg/g for all fractions except
the CBD resins, for which LLMV was 0.020 μg/g. Flutianil-treated
samples from nine field sites were collected from several crop production
regions and analyzed to determine the distribution of incurred flutianil
and OC56635 residues within the different hemp matrices. This data
was generated in support of nationwide registration with the United
States Environmental Protection Agency (USEPA).