Magnetic C60 nanospheres based solid-phase extraction coupled with isotope dilution gas chromatography-mass spectrometry method for the determination of sixteen polycyclic aromatic hydrocarbons in Chinese herbal medicines.

C60-based magnetic nanospheres were synthesized by coating Fe3O4 nanospheres with silica, then modifying with 3-aminopropyltriethoxysilane as a linker and a C60 fullerene stationary phase. The morphologies, magnetic properties, infrared absorption and carbon content of magnetic nanospheres were studied by TEM, VSM, FTIR and carbon and sulfur analyzer. The magnetic nanospheres were employed for the magnetic solid-phase extraction (MSPE) of 16 polycyclic aromatic hydrocarbons (PAHs) in nine Chinese herbal medicines. The analyses were conducted by isotope dilution gas chromatography-mass spectrometry. The main parameters influencing the extraction, including extraction solvent, adsorbent amount, and extraction time were optimized. Method validation showed that the limit of detection (LOD) was 0.02-0.11 µg/kg, and the limit of quantification (LOQ) was 0.07-0.36 µg/kg. The spiked recoveries rates for 16 PAHs in white peony root were 84.7-107.2%. The relative standard deviation (RSD) was 1.7-8.4%. The established method was further used for the determination 16 PAHs in nine Chinese herbal medicines. Total content of 16 PAHs varied from 73.6 µg/kg (fructus lycii) to 2172.6 µg/kg (astragalus root). The results indicate that the pollution of PAHs in Chinese herbal medicines is serious. The established method can effective detect PAHs contamination in Chinese herbal medicines.

Magnetic solid-phase extraction based on [60]fullerene functionalization of magnetic nanoparticles for the determination of sixteen polycyclic aromatic hydrocarbons in tea samples.

[60]Fullerene functionalized magnetic nanoparticles (Fe3O4@SiO2@C60) were prepared and characterized by transmission electron microscope, vibrating sample magnetometer and infrared spectroscopy. The Fe3O4@SiO2@C60 was then applied for the magnetic solid-phase extraction of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in tea samples. The analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Parameters affecting the extraction, including sorbent amount, desorption solvent, salt concentration, pH and extraction time were investigated. Under optimized conditions, the developed method based on Fe3O4@SiO2@C60 gave detection limits of 0.8-14.3 ng L-1, and quantification limits of 2.6-47.6 ng L-1 for 16 PAHs, respectively. The spiked recoveries of the target PAHs in tea samples ranged from 92.4% to 106.9%. The intra-day and inter-day relative standard deviations (RSDs) were lower than 8.7% and 10.6%, respectively. These results demonstrated that the established method could be applied to the analysis of PAHs at trace level in tea samples.