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ANALYTICAL METHODS: Chlorothalonil and degradates – Sediments

Extraction of chlorothalonil and three of its degradates from sediment and soils by a single method with analysis via gas chromatography-mass spectrometry

Hladik, M.L. and Kuivila, K.M., 2008,, J. Agric. Food Chem., v. 56, 2310–2314

A method has been developed for the simultaneous extraction of chlorothalonil and three of its degradates (4-hydroxy-2,5,6-trichloroisophthalonitrile, 1-carbamoyl-3-cyano-4-hydroxy-2,5,6-trichlorobenzene, and 1,3-dicarbamoyl-2,4,5,6-tetrachlorobenzene) from soils and sediments; the compounds were extracted using sonication with acetone and isolation of the parent compound and matrix interferences from the degradates by solid phase extraction (SPE). The chlorothalonil fraction underwent further coextracted matrix interference removal with Florisil. The degradates were derivatized with N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). All compounds were analyzed by gas chromatography–mass spectrometry (GC-MS). Recoveries on a spiked (20 and 200 µg/kg) sediment ranged from 80% to 91% with calculated limits of detection of 1-5 µg/kg dry weight sediment. An additional 20 sediment samples were collected in watersheds from the Southeastern United States where chlorothalonil is used widely on peanuts and other crops. None of the target compounds were detected. Laboratory fortified recoveries of chlorothalonil and its degradates in these environmental sediment samples ranged from 75% to 89%.


Compound
Recovery ±
Limit of Detection 
Limit of Quantitation 
RSD (%)
(µg/kg)
(µg/kg)
Chlorothalonil
91 ± 4
1
3
4-hydroxy-2,5,6-trichloroisophthalonitrile
86 ± 6
5
15
1-carbamoyl-3-cyano-4-hydroxy-2,5,6-trichlorobenzene
82 ± 6 
2
6
1,3-dicarbamoyl-2,4,5,6-tetrachlorobenzene
80 ± 5
2
6




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