Determination of coumarin anticoagulant rodenticide residues in animal tissue by high-performance liquid chromatography. I. Fluorescence detection using post-column techniques.
A multi-residue method was developed for the determination of the rodenticides warfarin, coumatetralyl, bromadiolone, difenacoum and brodifacoum in animal tissues by high-performance liquid chromatography with fluorescence detection. Extracts were cleaned-up by gel permeation chromatography on Bio-Beads SX-3 and residues determined by normal and reversed-phase high-performance liquid chromatography using post-column pH-switching, with chloroform -sec.-butylamine and borate buffer (pH 10.4) respectively, to maximise the native fluorimetric responses. Confirmation of identification was possible by re-chromatographing extracts in the absence of the post-column reagent. Chloroform-acetone (1:1) was significantly better than chloroform for the extraction of residues of these rodenticides from liver tissues. Recoveries from spiked liver tissue were generally greater than 90% at levels of 0.05-1 mg kg-1. Detection limits in animal tissues of 0.002 mg kg-1 for coumatetratyl, difenacoum and brodifacoum, 0.01 mg kg-1 for bromadiolone and 0.02 mg kg-1 for warfarin and could be routinely achieved.
D000818:Animals; D002415:Cats; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D003374:Coumarins / Q000032:analysis*; D004285:Dogs; D010573:Pesticide Residues / Q000032:analysis*; D011200:Poultry; D012378:Rodenticides / Q000032:analysis*; D013050:Spectrometry, Fluorescence / Q000379:methods
D003374:Coumarins; D010573:Pesticide Residues; D012378:Rodenticides