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J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Apr 1;955-956:86-92. doi: 10.1016/j.jchromb.2014.02.012. Epub 2014 Feb 19.

Determination of Celecoxib in human plasma using liquid chromatography with high resolution time of flight-mass spectrometry.

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Department of Chemistry, University of North Dakota, 151 Cornell Street, Grand Forks, ND 58202, USA.
School of Medicine and Health Sciences University of North Dakota, 501 N Columbia Rd. Grand Forks, ND 58203, USA.
Chemical Engineering Department, College of Engineering and Mines, University of North Dakota, 241 Centennial Dr., Grand Forks, ND 58202, USA.
Department of Chemistry, University of North Dakota, 151 Cornell Street, Grand Forks, ND 58202, USA. Electronic address:


A sensitive method for the determination of Celecoxib (CXB) in human plasma samples was developed using liquid chromatography coupled to electrospray ionization and time of flight mass spectrometry (LC-ESI-TOF-MS). A full factorial design of experiments (FF-DOE) methodology was applied to optimize the ESI conditions for CXB determination and also to predict the effects of interactions of multiple parameters affecting ionization (i.e., capillary voltage, fragmentor voltage, electrolyte and electrolyte concentration). The optimum ionization voltages were 4500V and 220V for capillary and fragmentor, respectively. Even though the highest ESI efficiency was obtained without electrolytes, the addition of 1.0mM ammonium acetate was shown to be essential to buffer the matrix effect and ensure a consistent response. In contrast to previous studies, deuterated CXB was used as a recovery (surrogate) standard, which enabled the correction of CXB loss during sample preparation. The extraction recovery using solid phase extraction was 87-98%. The instrumental limit of detection of CXB (LOD), 0.33ng/mL, and matrix affected LOD, 0.55ng/mL, were similar and comparable to the previously reported LC-MS/MS LODs. This method was employed to determine CXB concentrations in human plasma samples. Upon administration of 400mg CXB to the healthy women, the concentrations found in the plasma were 440-3300ng/mL. The inter-day repeatability was less than 4% RSD.


Celecoxib; ESI; Full factorial design; HPLC; Human plasma; TOF

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