title: Sol-gel-derived magnetic SiO2/TiO2nanocomposite reinforced hollow fiber-solid phase microextraction for enrichment of non-steroidal anti-inflammatory drugs from human hair prior to high performance liquid chromatography.
abstract: Hollow fiber-solid phase micro-extraction (HF-SPME) technique containing sol-gel-derived Fe3O4/SiO2/TiO2core-double shell nanocomposite as a novel high efficiency sorbent, coupled with high performance liquid chromatography was used to extraction and determination of six non-steroidal anti-inflammatory drugs; acetylsalicylic acid, naproxen, piroxicam, diclofenac, indomethacin and mefenamic acid, in hair samples. First, magnetite nanoparticles (Fe3O4-NPs) were synthesized by chemical co-precipitation of Fe(II) and Fe(III) ions (where the ratio of Fe(II) to Fe(III) is 1:2 and a non-oxidizing environment), in alkaline medium to produce magnetite particles. Subsequently, surface of Fe3O4-NPs was modified with SiO2and TiO2using layer-by-layer chemical technique. A core-shell structure of Fe3O4/SiO2/TiO2composite was prepared by coating magnetite core particles with silica and titania layers. In the proposed method, NSAIDs were extracted by the synthesized nanocomposite and analyzed by HPLC. The parameters affecting the efficiency of magnetic nanoparticle (MNPs) assisted HF-SPME were investigated and optimized. The method validation was included and satisfying results with high pre-concentration factors (405 up to 2450) were obtained. It owes large surface area and porosity of the nano-adsorbent. Under the optimal conditions, the method detection limits (S/N=3) were in the range of 0.01-0.10μgml-1and the limits of quantification (S/N=10) between 0.04 and 0.30μgml-1. Relative standard deviations were 3.09-6.61%. Eventually, the method was successfully applied to human hair after administration of NSAIDs.
authors.affiliation: Department of Chemistry, Payame Noor University, 19395-4697 Iran. Electronic address: eshaghi@pnu.ac.ir.
authors.forename: Zarrin
authors.initials: Z
authors.lastname: Es'haghi
authors.affiliation: Department of Chemistry, Payame Noor University, 19395-4697 Iran.
authors.forename: Effat
authors.initials: E
authors.lastname: Esmaeili-Shahri
keywords: Fe(3)O(4)/SiO(2)/TiO(2) nano composite; Hair sample; Hollow-fiber solid-phase micro-extraction (HF-SPME); Non-steroidal anti-inflammatory drugs; Sol–gel