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Method for determination of acephate, methamidophos, omethoate, dimethoate, ethylenethiourea and propylenethiourea in human urine using high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry

Journal of Exposure Science & Environmental Epidemiology volume 17, pages 321–330 (2007)Cite this article

Abstract

Because of increasing concern about widespread use of insecticides and fungicides, we have developed a highly sensitive analytical method to quantify urine-specific urinary biomarkers of the organophosphorus pesticides acephate, methamidophos, omethoate, dimethoate, and two metabolites from the fungicides alkylenebis-(dithiocarbamate) family: ethylenethiourea and propylenethiourea. The general sample preparation included lyophilization of the urine samples followed by extraction with dichloromethane. The analytical separation was performed by high-performance liquid chromatography (HPLC), and detection by a triple quadrupole mass spectrometer with and atmospheric pressure chemical ionization source in positive ion mode using multiple reaction monitoring and tandem mass spectrometry (MS/MS) analysis. Two different Thermo-Finnigan (San Jose, CA, USA) triple quadrupole mass spectrometers, a TSQ 7000 and a TSQ Quantum Ultra, were used in these analyses; results are presented comparing the method specifications of these two instruments. Isotopically labeled internal standards were used for three of the analytes. The use of labeled internal standards in combination with HPLC-MS/MS provided a high degree of selectivity and precision. Repeated analysis of urine samples spiked with high, medium and low concentration of the analytes gave relative standard deviations of less than 18%. For all compounds the extraction efficiency ranged between 52% and 63%, relative recoveries were about 100%, and the limits of detection were in the range of 0.001–0.282 ng/ml.

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Author notes

  1. Anders O Olsson

    Present address: AstraZeneca R&D Mölndal, Mölndal, Sweden

Authors and Affiliations

  1. Centers for Disease Control and Prevention, 4770 Buford Hwy NE, Mailstop F-17, Atlanta, 30341, Georgia, USA

    M Angela Montesano, Anders O Olsson, Peter Kuklenyik, Larry L Needham & Dana B Barr

  2. Center for Children's Environmental Health Research, School of Public Health, University of California, Berkeley, 94720-7360, California, USA

    A S A Bradman

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  1. M Angela Montesano
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  2. Anders O Olsson
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  3. Peter Kuklenyik
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  4. Larry L Needham
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Corresponding author

Correspondence to M Angela Montesano.

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The views expressed in this paper are those of the authors and do not necessarily reflect the views or policies of the Centers for Disease Control and Prevention. The authors state no competing financial interests.

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Montesano, M., Olsson, A., Kuklenyik, P. et al. Method for determination of acephate, methamidophos, omethoate, dimethoate, ethylenethiourea and propylenethiourea in human urine using high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry. J Expo Sci Environ Epidemiol 17, 321–330 (2007). https://doi.org/10.1038/sj.jes.7500550

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