ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Cloud point extraction combined with HPLC–MS for the determination of nimesulide in biological samples

Oksana G. Makukha, Lilia A. Ivashchenko, Olga A. Zaporozhets, and Volodymyr O. Doroschuk

Taras Shevchenko National University of Kyiv, Kyiv, Ukraine

E-mail: Makukhaoksana@gmail.com

Abstract: A high performance liquid chromatography (HPLC) method with mass spectrometry (MS) detection coupled previously cloud point preconcentration was developed for the determination of nimesulide in synthetic urine. Non-ionic surfactants Triton X-100 and Triton X-114 were used for cloud point extraction (CPE) of nimesulide. Various influencing parameters on the CPE process, such as pH, the concentration of non-ionic surfactant, equilibration temperature, incubation time and centrifugation parameters were studied and optimized. The developed method was validated; the linear range was in the range 67–5000 ng mL⁻¹, the detection (3σ) and quantification (10σ) limits were 20 ng mL⁻¹ and 67 ng mL⁻¹, respectively. The intra-day and inter-day precisions were less than 14%, the average recovery factors were in the range 95–117%. The suggested CPE–HPLC–MS method was simple and sensitive and could be an effective tool for the determination of nimesulide in biological samples.

Keywords: Cloud point extraction ; Nimesulide determination ; Non-ionic surfactant 

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-018-0618-0

Chemical Papers 73 (3) 693–699 (2019)