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Method for analysis of methyltetrahydrophthalic acid in urine using gas chromatography and selected ion monitoring

Lindh, Christian LU and Jönsson, Bo A LU (1994) In Journal of chromatography. B, Biomedical applications 660(1). p.57-66
Abstract
A method for the determination of methyltetrahydrophthalic acid (MTHP acid), a metabolite of methyltetrahydrophthalic anhydride (MTHPA) in human urine, was developed. The investigated MTHP acid was obtained by hydrolysis of a commercial MTHPA mixture, composed of three major isomers. These were synthesized and identified as 3-methyl-delta 4-tetrahydrophthalic anhydride, 4-methyl-delta 4-tetrahydrophthalic anhydride and 4-methyl-delta 3-tetrahydrophthalic anhydride. The urine was worked up by a liquid-solid extraction technique using C18 sorbent columns. Esterification was performed with methanol and boron trifluoride. The derivative in toluene was analyzed with capillary gas chromatography and selected ion monitoring. Deuterium-labeled... (More)
A method for the determination of methyltetrahydrophthalic acid (MTHP acid), a metabolite of methyltetrahydrophthalic anhydride (MTHPA) in human urine, was developed. The investigated MTHP acid was obtained by hydrolysis of a commercial MTHPA mixture, composed of three major isomers. These were synthesized and identified as 3-methyl-delta 4-tetrahydrophthalic anhydride, 4-methyl-delta 4-tetrahydrophthalic anhydride and 4-methyl-delta 3-tetrahydrophthalic anhydride. The urine was worked up by a liquid-solid extraction technique using C18 sorbent columns. Esterification was performed with methanol and boron trifluoride. The derivative in toluene was analyzed with capillary gas chromatography and selected ion monitoring. Deuterium-labeled MTHP acid was used as internal standard. The intra-assay precision for the overall method was between 4 and 8% in the range 3-110 ng/ml and the inter-assay precision was between 4 and 7% in the range 30-110 ng/ml. The total recoveries of the MTHP acid at 19 and 190 ng/ml were 94 and 97%, respectively. The total detection limit for the three isomers was < 6 ng/ml. Analysis of urine from a worker exposed to MTHPA makes it reasonable to assume that the method may be used for biological monitoring of MTHPA exposure. (Less)
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author
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of chromatography. B, Biomedical applications
volume
660
issue
1
pages
57 - 66
publisher
Elsevier
external identifiers
  • pmid:7858724
  • scopus:0027959580
ISSN
1572-6495
DOI
10.1016/0378-4347(94)00271-1
language
English
LU publication?
yes
id
93ec8e99-663d-4cd3-90af-8ee47c3c1574 (old id 1107879)
date added to LUP
2008-07-23 09:15:28
date last changed
2017-07-30 04:28:42
@article{93ec8e99-663d-4cd3-90af-8ee47c3c1574,
  abstract     = {A method for the determination of methyltetrahydrophthalic acid (MTHP acid), a metabolite of methyltetrahydrophthalic anhydride (MTHPA) in human urine, was developed. The investigated MTHP acid was obtained by hydrolysis of a commercial MTHPA mixture, composed of three major isomers. These were synthesized and identified as 3-methyl-delta 4-tetrahydrophthalic anhydride, 4-methyl-delta 4-tetrahydrophthalic anhydride and 4-methyl-delta 3-tetrahydrophthalic anhydride. The urine was worked up by a liquid-solid extraction technique using C18 sorbent columns. Esterification was performed with methanol and boron trifluoride. The derivative in toluene was analyzed with capillary gas chromatography and selected ion monitoring. Deuterium-labeled MTHP acid was used as internal standard. The intra-assay precision for the overall method was between 4 and 8% in the range 3-110 ng/ml and the inter-assay precision was between 4 and 7% in the range 30-110 ng/ml. The total recoveries of the MTHP acid at 19 and 190 ng/ml were 94 and 97%, respectively. The total detection limit for the three isomers was &lt; 6 ng/ml. Analysis of urine from a worker exposed to MTHPA makes it reasonable to assume that the method may be used for biological monitoring of MTHPA exposure.},
  author       = {Lindh, Christian and Jönsson, Bo A},
  issn         = {1572-6495},
  language     = {eng},
  number       = {1},
  pages        = {57--66},
  publisher    = {Elsevier},
  series       = {Journal of chromatography. B, Biomedical applications},
  title        = {Method for analysis of methyltetrahydrophthalic acid in urine using gas chromatography and selected ion monitoring},
  url          = {http://dx.doi.org/10.1016/0378-4347(94)00271-1},
  volume       = {660},
  year         = {1994},
}