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

  • Volodymyr O. Doroschuk EMAIL logo , Anastasiya B. Grogul , Yevhen S. Mandzyuk , Oksana G. Makukha und Nataliya O. Grytsyk
Veröffentlicht/Copyright: 25. Juni 2016
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Abstract

A new simple cloud point extraction/preconcentration method was developed for the HPLC-MS/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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Received: 2015-12-21
Revised: 2016-3-10
Accepted: 2016-3-11
Published Online: 2016-6-25
Published in Print: 2016-10-1

© 2016 Institute of Chemistry, Slovak Academy of Sciences

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