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Analysis of ethylenethiourea as a biomarker in human urine using liquid chromatography/triple quadrupole mass spectrometry.

Lindh, Christian LU ; Littorin, Margareta LU ; Johannesson, Gunvor LU and Jönsson, Bo A LU (2008) In Rapid Communications in Mass Spectrometry 22(16). p.2573-2579
Abstract
Ethylenebisdithiocarbamates (EBDCs) are widely used fungicides. Ethylenethiourea (ETU), the main metabolite and also a contaminant in the commercially available products, is of major toxicological concern. In this study, a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) is described for the analysis of ETU in human urine after a single-step extractive derivatization using pentafluorobenzyl bromide (PFBBr). Analysis was carried out using selected reaction monitoring (SRM) in the positive ion mode. Quantification of ETU was performed using [(2)H(4)]-labeled ETU as internal standard (IS). The limit of detection (LOD) was determined to 0.05 ng/mL. The method was linear in the range 0.1-54 ng/mL urine and had a... (More)
Ethylenebisdithiocarbamates (EBDCs) are widely used fungicides. Ethylenethiourea (ETU), the main metabolite and also a contaminant in the commercially available products, is of major toxicological concern. In this study, a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) is described for the analysis of ETU in human urine after a single-step extractive derivatization using pentafluorobenzyl bromide (PFBBr). Analysis was carried out using selected reaction monitoring (SRM) in the positive ion mode. Quantification of ETU was performed using [(2)H(4)]-labeled ETU as internal standard (IS). The limit of detection (LOD) was determined to 0.05 ng/mL. The method was linear in the range 0.1-54 ng/mL urine and had a within-run precision of 3-5%. The between-run precision was determined at an average urine level of 2 and 10 ng/mL urine and found to be 9%. The inter-batch precision was 6%. To validate ETU as a biomarker of exposure, the method was applied in a human experimental oral exposure to the commercial fungicide Ridomil Gold, containing 64% mancozeb and 4.5% ETU. Two healthy volunteers received 8.9 microg/kg body weight (b.w.) Ridomil Gold in a single oral dose followed by urine sampling for 104 h post-exposure. The elimination half-life of ETU was estimated to 17-23 h. (Less)
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author
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Rapid Communications in Mass Spectrometry
volume
22
issue
16
pages
2573 - 2579
publisher
John Wiley & Sons
external identifiers
  • wos:000258627400023
  • pmid:18651716
  • scopus:50249185527
ISSN
1097-0231
DOI
10.1002/rcm.3647
language
English
LU publication?
yes
id
2b7d10e2-c8a3-4980-8268-ba59b8823f51 (old id 1180883)
alternative location
http://www.ncbi.nlm.nih.gov/pubmed/18651716?dopt=Abstract
date added to LUP
2008-09-10 17:42:10
date last changed
2017-01-22 03:31:57
@article{2b7d10e2-c8a3-4980-8268-ba59b8823f51,
  abstract     = {Ethylenebisdithiocarbamates (EBDCs) are widely used fungicides. Ethylenethiourea (ETU), the main metabolite and also a contaminant in the commercially available products, is of major toxicological concern. In this study, a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) is described for the analysis of ETU in human urine after a single-step extractive derivatization using pentafluorobenzyl bromide (PFBBr). Analysis was carried out using selected reaction monitoring (SRM) in the positive ion mode. Quantification of ETU was performed using [(2)H(4)]-labeled ETU as internal standard (IS). The limit of detection (LOD) was determined to 0.05 ng/mL. The method was linear in the range 0.1-54 ng/mL urine and had a within-run precision of 3-5%. The between-run precision was determined at an average urine level of 2 and 10 ng/mL urine and found to be 9%. The inter-batch precision was 6%. To validate ETU as a biomarker of exposure, the method was applied in a human experimental oral exposure to the commercial fungicide Ridomil Gold, containing 64% mancozeb and 4.5% ETU. Two healthy volunteers received 8.9 microg/kg body weight (b.w.) Ridomil Gold in a single oral dose followed by urine sampling for 104 h post-exposure. The elimination half-life of ETU was estimated to 17-23 h.},
  author       = {Lindh, Christian and Littorin, Margareta and Johannesson, Gunvor and Jönsson, Bo A},
  issn         = {1097-0231},
  language     = {eng},
  number       = {16},
  pages        = {2573--2579},
  publisher    = {John Wiley & Sons},
  series       = {Rapid Communications in Mass Spectrometry},
  title        = {Analysis of ethylenethiourea as a biomarker in human urine using liquid chromatography/triple quadrupole mass spectrometry.},
  url          = {http://dx.doi.org/10.1002/rcm.3647},
  volume       = {22},
  year         = {2008},
}