Journal article
Identification of N-methylsaccharin as a peak at the retention time of methylated (2,4,5-trichlorophenoxy)acetic acid in human urinary exposure samples
Journal of agricultural and food chemistry, Vol.30(6), pp.1256-1258
11/01/1982
DOI: 10.1021/jf00114a065
Abstract
Human exposure to (2,4,5-trichlorophenoxy)acetic acid (2,4,5-T) may be detected by analysis of a 24–48 h postexposure urine sample. Acid hydrolysis of the urine followed by extraction with benzene and methylation of the extract with diazomethane will yield a gas chromatographic peak when a 6 ft long by 4 mm i.d. 4% SE-30/6% OV-210 column is used that matches that of a similarly treated standard of 2,4,5-T. Evidence is shown that N-methylsaccharin has an almost identical retention time and can be confused with 2,4,5-T methyl ester. Saccharin in diet drinks provides adequate amounts of urine saccharin for detection. GC/MS confirmation analysis supports the identification of N-methylsaccharin at the same retention time. Alternate columns can be used to detect 2,4,5-T exposure by using the same hydrolysis and extraction procedure. These would include a 6 ft long × 4 mm i.d. 1.5% OV-17/1.95% OV-210 and a 15 ft long by 4 mm i.d. SE-30/OV-210 column, both of which resolve the 2,4,5-T and saccharin peaks. Human exposure to 2,4,5-T is frequently determined by use of a modified Bevenue procedure (Bevenue et al., 1968) as described by Rivers et al. (1970). The procedure requires the benzene extraction of an acid-hydrolyzed urine or blood sample, followed by methylation of the extract with diazomethane. Determination is by electron-capture GC. Of the several options for column selection in the GC determination, it is frequently a choice of the analyst to use 4% SE-30/6% OV-210 as the liquid phase because of its general applicability to pesticide chemistry (Watts, 1980). This paper will describe work wherein an analyst can easily report a false positive for 2,4,5-T when the compound may actually be N-methylsaccharin [2-methyl-1,2-benzisothiazol-3(2H)-one 1,1-dioxide]. Diet drinks commonly yield enough saccharin in the urine so that a strong indication of 2,4,5-T could easily be suggested if a 6 ft long SE-30/OV-210 column is used for GC separation of peaks. Obviously, other column selections should be made, and the present work describes some successful alternatives. © 1982, American Chemical Society. All rights reserved.
Details
- Title: Subtitle
- Identification of N-methylsaccharin as a peak at the retention time of methylated (2,4,5-trichlorophenoxy)acetic acid in human urinary exposure samples
- Creators
- Kenneth W KirbyHerbert L HetzlerEdwin F SlachDavid F WiemerMichael J Aaronson
- Resource Type
- Journal article
- Publication Details
- Journal of agricultural and food chemistry, Vol.30(6), pp.1256-1258
- Publisher
- American Chemical Society
- DOI
- 10.1021/jf00114a065
- ISSN
- 0021-8561
- eISSN
- 1520-5118
- Language
- English
- Date published
- 11/01/1982
- Academic Unit
- Neuroscience and Pharmacology; Chemistry
- Record Identifier
- 9984216667802771
Metrics
1 Record Views