Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1614, Issue -, Pages -Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2019.460718
Keywords
Electrospinning; Micro solid phase extraction by packed sorbent; Nylon 6; Layered double hydroxide; Non-steroidal anti-inflammatory drugs; Blood
Funding
- K.N. Toosi University of Technology
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In the present work, NiFe layered double hydroxide (LDH)/Nylon 6 composite nanofibers were prepared by electrospinning method and used as a new sorbent for the extraction and measurement of nonsteroidal anti-inflammatory drugs (naproxen, mefenamic acid, and diclofenac) in whole blood samples. The method is based on micro solid phase extraction (mu SPE) by packed sorbent followed by HPLC-UV analysis. Effective parameters on the extraction efficiency were optimized using a central composite design (CCD). In order to characterize the sorbent, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDX) and elemental mapping were applied. The method was fully validated based on linearity, limits of detection (LOD) and quantification (LOQ), precision, and recovery. Under the optimal conditions, LOD values were found to be 25 ng mL(-1) for naproxen and diclofenac and 15 ng mL -1 for mefenamic acid. A seven-point calibration curve was obtained in the range of 75-2000 ng mL(-1) for naproxen and diclofenac and 50-2000 for mefenamic acid. The method showed good linearity with coefficients of determination, r(2) > 0.9962, for the three drugs. In the entire analytical range, the relative standard deviations (RSD%) were less than 8.1%. Finally, the efficiency of the method was investigated for the analysis of the target analytes in human blood samples, and the recoveries were obtained in the range of 90.7-109.8%. (C) 2019 Elsevier B.V. All rights reserved.
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