ISSN print edition: 0366-6352
ISSN electronic edition: 1336-9075
Registr. No.: MK SR 9/7
Cloud point extraction of disulfiram for its HPLC-MS/MS determination in synthetic urine
Volodymyr O. Doroschuk, Anastasiya B. Grogul, Yevhen S. Mandzyuk, Oksana G. Makukha, and Nataliya O. Grytsyk
Analytical Chemistry Department, Faculty of Chemistry, Taras Shevchenko Kyiv University, Volodymyrska Str. 64, Kyiv, 01033, Ukraine
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.
Keywords: cloud point extraction – disulfiram determination – non-ionic surfactant
Full paper is available at www.springerlink.com.
Chemical Papers 70 (10) 1316–1321 (2016)