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  • Title: Nickel-iron layered double hydroxide nanostructures for micro solid phase extraction of nonsteroidal anti-inflammatory drugs, followed by quantitation by HPLC-UV.
    Author: Seidi S, Sanàti SE.
    Journal: Mikrochim Acta; 2019 Apr 23; 186(5):297. PubMed ID: 31016399.
    Abstract:
    Layered double hydroxides (LDHs) of nickel and iron were hydrothermally prepared by co-precipitation using urea hydrolysis. The Ni-Fe LDH nanostructures were characterized by X-ray diffraction, FT-IR spectroscopy, scanning electron microscopy, thermogravimetric and energy dispersive X-ray analysis. The LDHs are shown to be a viable sorbent for micro solid phase extraction by packed sorbent of the nonsteroidal anti-inflammatory drugs (NSAIDs) diclofenac, ibuprofen, mefenamic acid and naproxen from human urine. Adsorption and desorption parameters were optimized using a central composite design. Following desorption with a methanol/water mixture (95:5 v:v) containing 0.1% formic acid, the NSAIDs were quantified by HPLC with UV detection. Under the optimal conditions, response is linear in the 10-1000 ng.mL-1 NSAID concentration range. Limits of detection and intra-day and inter-day RSDs are <10 ng.mL-1 and 10.2%, respectively. The method was successfully applied to the determination of NSAIDs in some positive human urine samples. Relative recoveries from spiked samples range from 94.8 to 113%. Graphical abstract Layered double hydroxides of nickel and iron were synthesized and packed in a spinal syringe for micro solid phase extraction of non-steroidal anti-inflammatory drugs.
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