Gas chromatographic determination of chlorothalonil and its metabolite 4-hydroxy-2,5,6-trichloroisophtalonitrile (HTI) in water

Summary A gas chromatographic method, with electron capture detection and mass spectrometric confirmation, is described for the determination of chlorothalonil and its metabolite 4-hydroxy-2,5,6-trichloroisophtalonitrile (HTI) in water samples. Water is saturated with sodium chloride and acidified to pH<2 with dilute sulfuric acid. After extraction with dichloromethane, HTI was methylated with diazomethane. The extract obtained was cleaned with basic alumina. Chlorothalonil and the methylated HTI-derivative were determined by gas chromatography with electron capture detection (GC-ECD) and confirmed by gas chromatography-mass spectrometry (GC-MS). The limit of detection, depending on the nature of the water samples is for both compounds between 0.01–0.03 g 1^–1 water. The average recovery in ground water is 87% for chlorothalonil and 82 % for HTI.