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Title

SIMULTANEOUS DETERMINATION OF PYRETHROIDS RESIDUES IN FRUIT AND VEGETABLE SAMPLES VIA SUPERCRITICAL FLUID EXTRACTION FOLLOWED BY NEW MAGNETIC SOLID PHASE EXTRACTION BASED ON IONIC LIQUID COUPLED WITH HPLC-UV

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Abstract

 RECENTLY MAGNETIC SOLID-PHASE EXTRACTION (MSPE), AS A NOVEL SPE METHOD, HAS BEEN INTRODUCED BASED ON THE USE OF MAGNETIC NANOPARTICLES (MNPS) [1]. MNPS CAN ACHIEVE A SHORTER ANALYSIS TIME, DUE TO THE MAGNETICALLY ASSISTED SEPARATION OF THESE PARTICLES FROM THESAMPLE AND THEREFORE, NO SAMPLE CENTRIFUGATION OR FILTRATION IS NEEDED AFTER TREATMENT [2]. IN PRESENT STUDY, A NOVEL MAGNETIC ADSORBENT MODIFIED WITH IONIC LIQUID (IL), FE3O4@SIO2@IL NANOPARTICLES, WERE FABRICATED BY A SIMPLE METHOD AND APPLIED FOR MAGNETIC SOLID-PHASE EXTRACTION (MSPE). THE PREPARED MAGNETIC NANOPARTICLES WERE CHARACTERIZED BY USING FOURIER TRANSFORM INFRARED (FT-IR) SPECTROSCOPY, SCANNING ELECTRON MICROSCOPY (SEM), THERMO GRAVIMETRIC ANALYSIS (TGA) AND VIBRATING SAMPLE MAGNETOMETER (VSM). SINCE THEN, AND AFTER SUPERCRITICAL FLUID EXTRACTION (SFE), THE NEW SORBENT WERE APPLIED FOR MSPE OF THREE PYRETHROID RESIDUES INCLUDING FENPROPATHRIN, CYHALOTHRIN, ANDFENVALERATE FROM FRUIT AND VEGETABLE SAMPLES. AFTERWARD, THE EXTRACTED PYRETHROID RESIDUES WERE INTRODUCED TO HIGH PERFORMANCE LIQUID CHROMATOGRAPHY -ULTRA VIOLET (HPLC-UV) FOR ULTRA-TRACE ANALYZING. A TAGUCHI ORTHOGONAL ARRAY (OA) EXPERIMENTAL DESIGN WITH AN OA16 (45) MATRIX WAS EMPLOYED FOR OPTIMIZATION THE EFFECTING PARAMETERS ON SFE CONDITIONS. IN ADDITION, THE ADSORPTION AND DESORPTION CONDITIONS IN MSPE WERE OPTIMIZED BY CHOOSING THE APPROPRIATE PARAMETERS.UNDER THE OPTIMAL CONDITIONS, GOOD LINEARITY AT 2.5-250MGL-1 (0.9941 £ R2 £0.9998) AND 0.3−5 MGKG-1 (0.9931 £ R2 £ 0.9994) GOOD PRECISION 3.2-6.5% AND5.1 - 8.4%, AND LIMITS OF DETECTION WERE OBTAINED 1MGL-1 AND 0.1MGKG-1 FOR MSPE AND SFE-MSPE, RESPECTIVELY. THE RESULTS SHOWED THAT THE PRESENT METHOD IS A SIMPLE, ACCURATE AND HIGH EFFICIENT APPROACH FOR THE DETERMINATION OF PYRETHROIDS IN THE FRUIT AND VEGETABLE SAMPLES.

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