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LC-MS/MS 法分析大麻基质中的氟虫腈和 OC56635 残留。

Analysis of Flutianil and OC56635 Residues in Hemp Cannabis Matrices by LC-MS/MS.

机构信息

Department of Environmental Toxicology, University of California Davis, One Shields Avenue, Davis, California 95616, United States.

出版信息

J Agric Food Chem. 2024 Aug 28;72(34):18872-18879. doi: 10.1021/acs.jafc.4c05103. Epub 2024 Aug 14.

DOI:10.1021/acs.jafc.4c05103
PMID:39140410
Abstract

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 CO 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).

摘要

本文介绍了测定噻唑烷类杀菌剂氟环唑(商品名:GATTEN)及其主要代谢物 OC56635 在大麻大麻基质中的分析方法。共测试了 9 种作物基质:全种子、纤维、花蕾、麻心、麻籽油、麻粉、麻粉、乙醇提取的 CBD 树脂(CBD-E)和超临界 CO 提取的 CBD 树脂(CBD-C)。CBD-E 和 CBD-C 作物馏分的加工是在内部使用本文详述的方法进行的。田间样品分析采用顺序提取、堆叠固相萃取(SPE)柱净化和蒸发来准备 LC-MS/MS 定量分析的样品。使用未经处理的大麻基质对每个馏分进行了至少三个水平的方法验证,除 CBD 树脂外,所有馏分的最低方法验证水平(LLMV)为 0.010 μg/g,对于 CBD 树脂,LLMV 为 0.020 μg/g。从几个大麻生产地区采集了来自 9 个田间地点的氟环唑处理样品,并进行了分析,以确定不同大麻基质中氟环唑和 OC56635 残留的分布。该数据是为支持在美国环境保护署(USEPA)进行全国注册而生成的。

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