Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles.

The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL(-1) with low detection limit of 0.03 ng mL(-1) were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

Application of dispersive liquid-liquid microextraction coupled with vortex-assisted hydrophobic magnetic nanoparticles based solid-phase extraction for determination of aflatoxin M1 in milk samples by sensitive micelle enhanced spectrofluorimetry.

An efficient, simple and fast low-density solvent based dispersive liquid-liquid microextraction (LDS-DLLME) followed by vortex-assisted dispersive solid phase extraction (VA-D-SPE) has been developed as a new approach for extraction and preconcentration of aflatoxin M1 in milk samples prior to its micelle enhanced spectrofluorimetic determination. In this LDS-DLLME coupled VA-D-SPE method, milk samples were first treated with methanol/water (80:20, v/v) after removing the fat layer. This solvent was directly used as the dispersing solvent in DLLME along with using 1-heptanol (as a low-density solvent with respect to water) as the extracting solvent. In VA-D-SPE approach, hydrophobic oleic acid modified Fe3O4 nanoparticles were used to retrieve the analyte from the DLLME step. It is considerably that the target of VA-D-SPE was 1-heptanol rather than the aflatoxin M1 directly. The main parameters affecting the efficiency of LDS-DLLME and VA-D-SPE procedures and signal enhancement of aflatoxin M1 were investigated and optimized. Under the optimum conditions, the method was linear in the range from 0.02 to 200 µg L(-1) with the correlation coefficient (R(2)) of 0.9989 and detection limit of 13 ng L(-1). The intra-day precision was 2.9 and 4.3% and the inter-day precision was 2.1 and 3.3% for concentration of 2 and 50 µg L(-1) respectively. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method.

Magnetically assisted solid phase extraction using Fe3O4 nanoparticles combined with enhanced spectrofluorimetric detection for aflatoxin M1 determination in milk samples.

A novel, facile and inexpensive solid phase extraction (SPE) method using ethylene glycol bis-mercaptoacetate modified 3-(trimethoxysilyl)-1-propanethiol grafted Fe(3)O(4) nanoparticles coupled with spectrofluorimetric detection was proposed for determination of aflatoxin M1 (AFM1) in liquid milk samples. The method uses the advantage fluorescence enhancement by ß-cyclodexterin complexation of AFM1 in 12% (v/v) acetonitrile-water and the remarkable properties of Fe(3)O(4) nanoparticles namely high surface area and strong magnetization were utilized to achieve high enrichment factor (57) and satisfactory extraction recoveries (91-102%) using only 100 mg of magnetic adsorbent. Furthermore, fast separation time of about 15 min avoids many time-consuming column-passing procedures of conventional SPE. The main factors affecting extraction efficiency including pH value, desorption conditions, extraction/desorption time, sample volume, and adsorbent amount were evaluated and optimized. Under the optimal conditions, a wide linear range of 0.04-8 ng mL(-1) with a low detection limit of 0.015 ng mL(-1) was obtained. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method.

Application of magnetic solid phase extraction for separation and determination of aflatoxins B 1 and B2 in cereal products by high performance liquid chromatography-fluorescence detection.

A simple and sensitive method based on the magnetic solid phase extraction with modified magnetic nanoparticles followed by high performance liquid chromatography with fluorescence detection has been developed for extraction and determination of aflatoxins B1 (AFB1) and B2 (AFB2) in cereal products. Magnetic nanoparticle coated with 3-(trimethoxysilyl)-1-propanthiol (TMSPT) and modified with 2-amino-5-mercapto-1,3,4-thiadiazole (AMT) was used as an antibody-free adsorbent. Under the optimal conditions, the calibration curves for AFB1 and AFB2 were linear in the ranges of 0.2-15 µg L(-1) and 0.04-3 µg L(-1), respectively. Detection limit was 0.041 µg L(-1) for AFB1 and 0.013 µg L(-1) for AFB2. The proposed method was successfully applied to the determination of AFB1 and AFB2 in spiked corn and rice samples with an average recovery of 93.5%. The results demonstrated that the developed method is simple, rapid, inexpensive, accurate and remarkably free from interference effects.

Enhanced spectrofluorimetric determination of aflatoxin M1 in liquid milk after magnetic solid phase extraction.

A simple and sensitive method using magnetic solid phase extraction (MSPE) followed by spectrofluorimetric detection has been developed for separation and determination of aflatoxin M1 (AFM1) in liquid milk. The method is based on the extraction of AFM1 on the modified magnetic nanoparticles (MMNPs) and subsequent derivatization of extracted AFM1 to AFM1 hemi-acetal derivative (AFM2a) by reaction with trifluoroacetic acid (TFA) for spectrofluorimetric detection. Magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol (TMSPT) and modified with 2-amino-5-mercapto-1,3,4-thiadiazole (AMT) were used as adsorbent in MSPE procedure. Influential parameters affecting the extraction efficiency were investigated and optimized. Under the optimum conditions the calibration curve for AFM1 determination showed good linearity in the range 0.030-10.0 µg L(-1) (R(2) = 0.9991). The repeatability and reproducibility (RSD%) for 0.050 µg L(-1) of AFM1 were 4.5% and 5.3%, respectively and limit of detection limit (S/N = 3) was estimated to be 0.010 µg L(-1). The developed method was successfully applied for extraction of AFM1 from spiked liquid milk and natural contaminated liquid milk. The good spiked recoveries ranging from 91.6% to 96.1% were obtained. The results demonstrated that the developed method is simple, inexpensive, accurate and remarkably free from interference effects.