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Cloud point extraction of disulfiram for its HPLC-MS/MS determination in synthetic urine

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Abstract

A new simple cloud point extraction/preconcentration method was developed for the HPLCMS/MS determination of disulfiram in synthetic urine. Some parameters with an effect on the extraction, such as the concentration of Triton X-114, pH influence, incubation time, equilibration temperature and centrifuging parameters, were studied and optimised. The method proposed for the HPLC-MS/MS determination of disulfiram in synthetic urine with preliminary cloud point extraction was validated. The calibration curve was linear in the range of 0.025–15.4 ng mL−1. The limits of detection (3σ) and quantification (10σ) were 0.008 ng mL−1 and 0.025 ng mL−1, respectively. The matrix effect (96 %), recovery of the extraction procedure (95 %) and overall “process efficiency” (91 %) were also estimated. The results show that the sensitivity, metrological characteristics, ecological safety, simplicity and convenience of the suggested procedure exceed its analogues based on extraction using organic solvents.

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Authors and Affiliations

  1. Analytical Chemistry Department, Faculty of Chemistry, Taras Shevchenko Kyiv University, Volodymyrska Str. 64, Kyiv, 01033, Ukraine

    Volodymyr O. Doroschuk, Anastasiya B. Grogul, Yevhen S. Mandzyuk & Oksana G. Makukha

  2. Faculté de Chimie de Strasbourg, Université de Strasbourg, 1 rue Blaise Pascal, 67070, Strasbourg Cedex, France

    Nataliya O. Grytsyk

Authors
  1. Volodymyr O. Doroschuk
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  2. Anastasiya B. Grogul
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  3. Yevhen S. Mandzyuk
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  4. Oksana G. Makukha
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  5. Nataliya O. Grytsyk
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Correspondence to Volodymyr O. Doroschuk.

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Doroschuk, V.O., Grogul, A.B., Mandzyuk, Y.S. et al. Cloud point extraction of disulfiram for its HPLC-MS/MS determination in synthetic urine. Chem. Pap. 70, 1316–1321 (2016). https://doi.org/10.1515/chempap-2016-0074

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  • DOI: https://doi.org/10.1515/chempap-2016-0074

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