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T.D. Hubert

Publications and source records attributed to T.D. Hubert.

4 recordsLinked to original sources

Determination of 3-trifluoromethyl-4-nitrophenol and 3-trifluoromethyl-4-nitrophenol glucuronide in edible fillet tissue of rainbow trout and channel catfish by solid-phase extraction and liquid chromatography

3-Trifluoromethyl-4-nitrophenol (TFM) is a pesticide used for the selective control of sea lampreys ( Petromyzon marinus ) in stream and river tributaries of the Great Lakes. To determine concentrations of TFM and TFM glucuronide in the edible fillet tissue of fish during sea lamprey control treatments, an analytical method was developed to determine the concentrations of these residues in rainbow trout ( Oncorhynchus mykiss ; RBT) and channel catfish ( Ictalurus punctatis ; CCF). Homogenized fillets were extracted with methanol–water (80 + 20). TFM and TFM glucuronide were isolated from coextractives by C 18 solid-phase extraction. TFM glucuronide was hydrolyzed to TFM by the addition of β-glucuronidase to the TFM glucuronide extract. The extracts were analyzed separately by liquid chromatography with UV–visible detection. Recoveries from TFM-fortified CCF and RBT tissues were 84.1 and 96.1%, respectively. The method detection limits (MDLs) are 2.4 ng/g for TFM-fortified tissues of CCF and 3 ng/g for those of RBT. Recoveries were 78.8 and 77%from TFM glucuronide-fortified CCF and RBT tissues, respectively. The MDLs for TFM glucuronide-fortified tissues are 3.5 and 6.9 ng/g for CCF and RBT, respectively.

Journal of AOAC International

Metabolism of niclosamide in sediment and water systems

A series of experiments analyzed the kinetics and mechanisms of [ 14C]niclosamide degradation. The aerobic aquatic metabolism of [ 14C]niclosamide was studied in nonsterile river water/sediment mixtures. Test systems, maintained under aerobic conditions, were treated with niclosamide and incubated in the dark at 25.0 ?? 1.0 ??C for 30 days. Half-lives of 4.9 and 5.4 days were calculated for the chlorosalicylic acid- and chloronitroaniline-labeled test systems, respectively. From 0 to 21 days after treatment (DAT), the only metabolism product observed in either test system was aminoniclosamide. At the final sampling interval, five peaks were resolved from the chlorosalicylic acid label, and three peaks were resolved from the chloronitroaniline label test substance. By 30 DAT, sediment-bound residues represented ???70% of the observed radioactivity. For the anaerobic aquatic metabolism of [14C]niclosamide, test systems were incubated under anaerobic conditions for 365 days. Half-lives of 0.65 day for the chlorosalicylic acid label and 2.79 days for the chloronitroaniline label were calculated. From 0 to 3 DAT, niclosamide was first transformed into aminoniclosamide. Aminoniclosamide is readily formed, as it was observed in the chlorosalicylic acid label 0 DAT sampling. Several minor metabolites were observed in the water and sediment extracts. None of these metabolites were formed to a significant amount until the parent niclosamide dissipated below the detection limit. Two of the byproducts from these metabolism studies are polar unknowns eluting at 3 and 5 min by HPLC, similar to the unknowns observed in aqueous photolysis studies.

Journal of Agricultural and Food Chemistry

Aqueous photolysis of niclosamide

The photodegradation of [ 14 C]niclosamide was studied in sterile, pH 5, 7, and 9 buffered aqueous solutions under artificial sunlight at 25.0 ± 1.0 °C. Photolysis in pH 5 buffer is 4.3 times faster than in pH 9 buffer and 1.5 times faster than in pH 7 buffer. In the dark controls, niclosamide degraded only in the pH 5 buffer. After 360 h of continuous irradiation in pH 9 buffer, the chromatographic pattern of the degradates was the same regardless of which ring contained the radiolabel. An HPLC method was developed that confirmed these degradates to be carbon dioxide and two- and four-carbon aliphatic acids formed by cleavage of both aromatic rings. Carbon dioxide was the major degradate, comprising ∼40% of the initial radioactivity in the 360 h samples from both labels. The other degradates formed were oxalic acid, maleic acid, glyoxylic acid, and glyoxal. In addition, in the chloronitroaniline-labeled irradiated test solution, 2-chloro-4-nitroaniline was observed and identified after 48 h of irradiation but was not detected thereafter. No other aromatic compounds were isolated or observed in either labeled test system.

Journal of Agricultural and Food Chemistry

Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., <14%), and sensitivity (method quantitation limit, <24 ng/g) for each analyte indicate the usefulness of this method for studies characterizing the depletion of benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

Journal of Chromatography A