Abstract

Carbon-based Fe3O4 nanocomposites (C/Fe3O4 NCs) were synthesized by a simple one-step hydrothermal method using waste pomelo peels as the carbon precursors. The characterization results showed that they had good structures and physicochemical properties. The prepared C/Fe3O4 NCs could be applied as excellent and recyclable adsorbents for magnetic solid phase extraction (MSPE) of 11 triazole fungicides in fruit samples. In the MSPE procedure, several parameters including the amount of adsorbents, extraction time, the type and volume of desorption solvent, and desorption time were optimized in detail. Under the optimized conditions, the good linearity (R2 > 0.9916), the limits of detection (LOD), and quantification (LOQ) were obtained in the range of 1–100, 0.12–0.55, and 0.39–1.85 μg/kg for 11 pesticides, respectively. Lastly, the proposed MSPE method was successfully applied to analyze triazole fungicides in real apple, pear, orange, peach, and banana samples with recoveries in the range of 82.1% to 109.9% and relative standard deviations (RSDs) below 8.4%. Therefore, the C/Fe3O4 NCs based MSPE method has a great potential for isolating and pre-concentrating trace levels of triazole fungicides in fruits.

Highlights

  • Triazole fungicides, which are typically comprised of a 1,2,4-triazole moiety, a hydroxy group, and substituted benzyl [1], have been employed as systemic fungicides because of their high capability to hinder the biosynthesis of steroid hormones [2]

  • The improper use of these compounds has resulted in undesirable residues on fruits, which increase the risk of transferring the residual pesticides from the skin of fruits to consumers’ body

  • The validation of the developed magnetic solid phase extraction (MSPE) gas chromatography-mass spectrometer (MSPE-GC-MS) method for analyzing triazole fungicides was evaluated under the optimized experimental conditions

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Summary

Introduction

Triazole fungicides, which are typically comprised of a 1,2,4-triazole moiety, a hydroxy (keto) group, and substituted benzyl [1], have been employed as systemic fungicides because of their high capability to hinder the biosynthesis of steroid hormones [2]. Due to the trace level concentrations of these compounds, an efficient sample preparation technique before detection is essential prior to instrumental measurement directly to obtain the reliable results. 4 nanomaterials from PPs as adInsotrhbisensttsudfoyr, MweSPeEmhpalosyneodt wyeatsbteeePnPsretpoorptreedp.are the carbon-based Fe3O4 nanocomposites (CIn/Fteh3iOs 4stuNdCys,)wbeyema psliomypedlewoanset-esPtePps thoypdrreopthaerermthael cmarebtohnod-ba(sseede FFei3gOur4ena1n).oScoumbspeqousietnestl(yC, /tFhee3O4 NCsp)rbepyaaresdimCp/Flee3oOn4e-NstCespwheyrderoutsheedrmasaal dmsoerthbeondts(sfeoer Feixgturarceti1n)g. OLlaestfluyn, gthiceidCe/Fsef3rOom NaCpsp-blea,spedeaMr, SoPraEnmge,thaondd wbansana samprleospo(sseeed,Fiwghuirceh1h).aLs aastglyr,etaht epCot/eFneti3aOl 4foNr Cisso-lbaatisnegd aMndSPpErem-ceotnhcoedntwraatsinpgrotrpaocseelde,vwelhs iochf thraiaszaolgereat potefnutniaglicfiodresisionlafrtuinitgs.and pre-concentrating trace levels of triazole fungicides in fruits. The diffraction peaks at 2θ = 30.3◦, 35.5◦, 43.3◦, 53.2◦, 57.2◦, and 62.8◦ corresponded to (220), (311),. The raman spectrum ofi1n2dicated that the peaks at 1357 cm−1 (D-band) and 1590 cm−1 (G-band) (see Figure 2B) were associated with sp and sp2dhifyfrbarcitdioiznepdeackasrbato2nθ[=163]0..3S°u, 3b5s.e5q°,u4e3n.3t°l,y5,3t.h2e°, m57o.2r°p, hanodlo6g2y.8°ocfoCrr/eFspeo3nOd4edNtCos(2w20a)s, (o3b11s)e,r(v40e0d),by SEM and TEM(s4u2.c2cA)e,ss(s5sf1uh1lol)y,wasnnydnit(nh44eF0sii)gzfeaudcreeutss2ioCnfg,FCae3/OfaF4ce[e1-3c6Oe],n4rteeNsrpeCdecsctiuwvbeeilcyre,swtaruhpcipctuhrorienx.diTmichaaetteresalmtyhaasntpFhsepe3eOrci4tcrnaualmnwoipintadhritcitcahlteeesdawvtheeraretage size of aboutth5e0pneamks. Based odnetrhiveataivbeosv[e20r]e,swuhltisc,htmheigrhetwhaevree ardicshorobxedygsoemn-ecobenntzaeinnoinidgcgormopuopusnodns bCy/uFsein3gOπ4-Nπ Cinstesruacrtfiaocne. , which made CBw/ahFsieecd3hOmo4naNdtheCeCs/aFdbeoi3svOpe4eNrresCseuslwdtsi,espltlheirensreeswoweleullrteiinorsincohlfuootrixopyngrfeaoncr-tcpicoranacltataiicnpaiplnaglipcgparltiociuoaptniso. no.n C/Fe3O4 NCs surface,

Effect of Activation Factor
Effect of Extraction Time and Adsorbent Amount
Effect of pH
Effect of Salinity
Effect of Desorption Agent Type
Effect of Desorption Solvent Volume and Desorption Time
Validation of the Method
Analysis of Real Samples
Comparison with Other Methods
Materials
Instruments
Sample Preparation and MSPE Procedure
Findings
Conclusions
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