Spectrofluorimetric determination of zearalenone using dispersive liquid–liquid microextraction coupled to micro-solid phase extraction onto magnetic nanoparticles

• Published in: RSC advances Vol. 4; no. 85; pp. 45065 - 45073
• Main Authors: Hashemi, Mahdi, Taherimaslak, Zohreh, Parvizi, Sara, Torkejokar, Mohammad
• Format: Journal Article
• Language: English
• Published: 01.01.2014
• Subjects: Acetonitrile; Calibration; Dispersion; Joining; Liquid-liquid extraction; Nanoparticles; Solvents; Zearalenone
• ISSN: 2046-2069; 2046-2069
• DOI: 10.1039/C4RA07684B

A new and sensitive method using dispersive liquid–liquid microextraction (DLLME) coupled to micro-solid phase extraction (μ-SPE) onto magnetic nanoparticles was developed for spectrofluorimetric determination of zearalenone (ZEN) in corn samples. In this study the solvent used to extract the analyte from a solid matrix, was then utilized as disperser solvent in the DLLME process. The DLLME was performed by injecting 3 mL of acetonitrile/water (8 : 2, v/v) (disperser) containing 320 μL of 1-heptanol (extraction solvent) into 30 mL of water sample. In the present DLLME-μ-SPE approach, hydrophobic magnetic nanoparticles were used to retrieve the extractant of 1-heptanol in the DLLME step. In fact the target of μ-SPE was the 1-heptanol rather than the ZEN. The ZEN was extracted from hydrophobic magnetic nanoparticles by stirring with 1 mL of acetonitrile for 4 min. Influential parameters affecting the extraction efficiency were investigated and optimized. Under the optimum conditions the calibration curve for ZEN determination showed good linearity in the range 0.51–300.0 μg L −1 ( R 2 = 0.9994) and the limit of detection ( S / N = 3) was estimated to be 0.25 μg L −1 . The intra-day and inter-day precision (RSD %) of ZEN were in the range of 2.7–4.1%. High recoveries ranging from 93.2 to 102.1% were obtained. The results demonstrated that the developed method is simple, inexpensive, accurate and remarkably free from interference effects. Also, this two-step method reclaimed the versatility of DLLME because the selection of the extraction solvent was not limited to the high density solvents.