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| Determination of 16 Polycyclic Aromatic Hydrocarbons in Alpinia Oxyphylla Miq by Gas Chromatography-Mass Spectrometry |
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| DOI： |
| KeyWord:gas chromatography-mass spectrometry(GC-MS) stable isotope internal standard method Alpinia oxyphylla Miq polycyclic aromatic hydrocarbon(PAHs) matrix effect |
| Author | Institution |
| SUN Xi-zhen,DU Jia-wei,QIAN Quan-quan，WU Ping-gu |
1.Hubei Key Lab of Quality and Safety of Traditional Chinese Medicine & Health Food,Huangshi,China;2.Zhejing Provincial Center for Disease Control and Prevention,Hangzhou,China |
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| Abstract: |
| An effective method was developed for the determination of 16 polycyclic aromatic hydrocarbons(PAHs) in Alpinia oxyphylla Miq based on gas chromatography-mass spectrometry(GC-MS).The samples were separated on a DB-EUPAH capillary chromatography column,detected by GC-MS with electron ionization source in selective ion mode,and quantified by stable isotope internal standard method.The optimal extraction conditions were as follows:2.0 g of sample was added with isotope standard solution,then mixed with absolute ethanol and water to dissolve,followed by addition of 10 mL n-hexane for extraction.The extract was firstly subjected to solid-phase extraction with a Florisil column,then saponified with KOH-ethanol solution,and extracted again by solid-phase extraction with a polycyclic aromatic hydrocarbon molecularly imprinted column,finally,eluted with 5 mL dichloromethane-n-hexane(1∶1,by volume).Results showed that the 16 PAHs presented good linear relationships in the concentration range of 1.0-200.0 μg/L with correlation coefficients(r2) not less than 0.992 5.The limits of detection were in the range of 0.3-1.0 μg/kg,and the limits of quantitation were 1.0-3.0 μg/kg.The average recoveries(n=6) for benzo［c］ fluorene(BcFL) ranged from 65.4% to 72.8%,with intra-day relative standard deviations(RSD,n=6) of 6.0%-7.4% and inter-day relative standard deviations(RSD,n=6) of 8.5%,respectively,while the average recoveries for the other 15 PAHs were in the range of 89.3%-116%,with intra-day RSDs(n=6) of 0.10%-6.1% and inter-day RSDs(n=6) of 1.2%-7.5%,respectively.The developed method showed excellent purification effect,sensitivity and high accuracy,and was suitable for the simultaneous determination of 16 PAHs in Alpinia oxyphylla Miq. |
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