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| Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe3O4@SiO2@NH2@C60 Magnetic Solid Phase Extraction |
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| DOI： |
| KeyWord:polycyclic aromatic hydrocarbons magnetic nanospheres C60 magnetic solid phase extraction/gas chromatography－mass spectrometry Chinese herbal medicines |
| Author | Institution |
| SONG Zhong-rong，ZHOU Xiang，JIANG Qing-xiang，YAN Zhi-hong，CAI Ying，LI Hui |
1. School of Pharmacy，Jiangxi University of Chinese Medicine，Nanchang ，China; 2. Institute of Traditional Chinese Medicine Health Industry，China Academy of Chinese Medical Sciences，Nanchang ，China |
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| Abstract: |
| A gas chromatography－mass spectrometry with magnetic solid phase extraction based on Fe3O4@SiO2@NH2@C60 magnetic nanocomposites was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons（PAHs） in Chinese herbal medicines in this paper．The composites were characterized by Fourier transform infrared spectroscopy，scanning electron microscopy and vibrating sample magnetometer to confirm the successful modification of C60．Meanwhile，adsorption experiments were conducted，which showed that the magnetic nanocomposites had a strong adsorption capacity and good stability，and the adsorption efficiency did not change significantly after 10 times of reuse．The effects of extraction solvent type，sorbent dosage，adsorption time，desorption solvent type and desorption time on the extraction efficiency for 16 PAHs in herbal samples were investigated．The results showed that the complete adsorption of 10 mg of sorbent on the targets could be achieved within 4 min．Under the optimal magnetic solid phase extraction conditions，there were good linear relationships for 16 PAHs in the range of 5－1 000 μg/L，with correlation coefficients（r2） of 0.994 0－0.999 9．The limits of detection and the limits of quantitation were in the range of 0.2－1.2 μg/kg and 0.8－3.9 μg/kg，respectively．The spiked recoveries at three levels ranged from 84.1% to 104%，with relative standard deviations（RSDs） of 0.70%－8.3%，intra-day RSDs of 0.20%－3.5% and inter-day RSDs of 2.2%－6.9%．The developed method could effectively reduce the interference on PAHs targets from complex matrices in Chinese herbal medicine samples，and provide an easy-to-operate，sensitive and accurate method reference for the determination of PAHs in Chinese herbal medicines. |
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