In this study, magnetic graphene nanocomposite Fe3O4/rGO was synthesized by facile one-pot solvothermal method. The nanocomposite was successfully used as magnetic solid phase extraction (MSPE) adsorbents for the determination of aflatoxins in edible vegetable oils through the π–π stacking interactions. MSPE parameters including the amount of adsorbents, extraction and desorption time, washing conditions, and the type and volume of desorption solvent were optimized. Under optimal conditions, good linear relationships were achieved. Limits of detection of this method were as low as 0.02 µg/kg and 0.01 µg/kg for aflatoxin B1 and B2, respectively. Finally, the magnetic graphene nanocomposite was successfully applied to aflatoxin analysis in vegetable oils. The results indicated that the recoveries of the B-group aflatoxins ranged from 80.4% to 106.0%, whereas the relative standard deviations (RSDs) were less than 8.1%. Owing to the simplicity, rapidity and efficiency, Fe3O4/rGO magnetic solid phase extraction coupled with high-performance liquid chromatography fluorescence with post-column photochemical derivatization (Fe3O4/rGO MSPE-HPLC-PCD-FLD) is a promising analytical method for routine and accurate determination of aflatoxins in lipid matrices.
By introducing long carbon-chain alkyl groups at the C-13 position of berberine and palmatine, 13-n-hexyl/13-n-octyl berberine and palmatine chloride analogues 4a–d were synthesized and examined by MTT assays for cytotoxic activity in seven human cancer cell lines (7701QGY, SMMC7721, HepG2, CEM, CEM/VCR, KIII, Lewis), yielding IC50 values of 0.02 ± 0.01–13.58 ± 2.84 μM. 13-n-Octyl palmatine (compound 4d) gave the most potent inhibitor activity, with an IC50 of 0.02 ± 0.01 μM for SMMC7721. In all cases, the 13-n-alkyl berberine and palmatine analogues 4a–d were more cytotoxic than berberine and palmatine. In addition, compounds 4a–d also exhibited more potent cytotoxicity than berberine and palmatine in mice with S180 sarcoma xenografted in vivo. The primary screening results indicated that the 13-n-hexyl/13-n-octyl berberine and palmatine analogues might be valuable source for new potent anticancer drug candidates.
This study established an immunoaffinity column for selective extraction of aflatoxins in agri-products. Specifically, the immunoaffinity column was developed by covalently coupling monoclonal antibody 1C11 against aflatoxins to amino-silica gel microparticles and then packing these into a cartridge. The extraction conditions were thoroughly optimized in terms of loading, washing and eluting solutions. Under the optimal conditions, the immunoaffinity column had a capacity of 200 ng of aflatoxins. The detection limits (S/N = 3) for aflatoxin G1, B1, G2 and B2 were 0.03, 0.07, 0.05 and 0.09 μg·kg−1, and the corresponding quantification limits (S/N = 10) were 0.10, 0.25, 0.18 and 0.30 μg·kg−1, respectively. The recoveries of aflatoxins in samples were 90.1%–104.4% and RSDs were <4.4%. The developed method was further applied to the determination of aflatoxins in peanut, vegetable oil and tea samples, and the results indicated that peanut (26.9%), vegetable oils (28.0%) and tea (5.3%) samples were contaminated with aflatoxins, with levels ranging from 0.49 to 20.79 μg·kg−1.