| 高效溶剂萃取－固相萃取/气相色谱－质谱法测定大气颗粒物中多环芳烃和有机磷阻燃剂 |
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| 基金项目:山东省重点研发计划项目（2020CXGC011402） |
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| 中文摘要:建立了高效溶剂萃取（HPSE）－固相萃取（SPE）/气相色谱－质谱（GC－MS）测定大气颗粒物中16种多环芳烃（PAHs）和15种有机磷阻燃剂（OPFRs）的方法。以正己烷－二氯甲烷（1∶1，体积比）溶液为萃取溶剂，萃取液旋转蒸发浓缩后经Florisil固相萃取柱净化，PAHs和OPFRs的洗脱溶剂分别为10 mL正己烷－二氯甲烷（1∶1）和10 mL乙酸乙酯，洗脱液浓缩定容后进行GC－MS测定。16种PAHs和15种OPFRs的线性范围为0.001 ~ 2.0 μg/mL，相关系数（r2）均大于0.99；检出限（LOD，S/N = 3）分别为0.10 ~ 10.00 μg/L和2.59 ~ 75.00 μg/L，定量下限（LOQ，S/N = 10）分别为0.33 ~ 33.33 μg/L和8.63 ~ 250.00 μg/L；平均回收率分别为73.0% ~ 98.0%和69.3% ~ 111%，相对标准偏差（RSD）分别为3.7% ~ 13%和2.5% ~ 17%。该方法适用于大气颗粒物样品中多环芳烃和有机磷阻燃剂的测定。 |
| 中文关键词:高效溶剂萃取 固相萃取 气相色谱－质谱法 多环芳烃 有机磷阻燃剂 大气颗粒物 |
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| Determination of PAHs and OPFRs in Atmospheric Particulate Matters by High Performance Solvent Extraction－Solid Phase Extraction/Gas Chromatography－Mass Spectrometry |
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| Abstract:Polycyclic aromatic hydrocarbons（PAHs） and organophosphorus flame retardants（OPFRs） are widespread and persistent organic pollutants in the environment．A high performance solvent extraction（HPSE）－solid phase extraction（SPE）/gas chromatography－mass spectrometry（GC－MS） was established for the determination of 16 PAHs and 15 OPFRs in atmospheric particulate matters．The extraction solvent of HPSE was n-hexane－dichloromethane（1∶1，by volume） solution．Meanwhile，other instrument parameters of HPSE（e.g．temperature and pressure） were also optimized．The extracts were concentrated by rotary evaporation，and then purified by Florisil solid phase extraction column．The eluents for PAHs and OPFRs were 10 mL of n-hexane－dichloromethane（1∶1） and 10 mL of ethyl acetate，respectively，and then the eluents were concentrated and determined by GC－MS．The linear ranges for 16 PAHs and 15 OPFRs were 0.001－2.0 μg/mL，and the correlation coefficients（r2） were greater than 0.99．The limits of detection（LODs，S/N = 3） for PAHs and OPFRs were 0.10－10.00 μg/L and 2.59－75.00 μg/L，respectively．The limits of quantitation（LOQs，S/N = 10） were 0.33－33.33 μg/L and 8.63－250.00 μg/L，respectively．The average recoveries for 16 PAHs and 15 OPFRs were in the range of 73.0%－98.0% and 69.3%－111%，with their relative standard deviations（RSDs） of 3.7%－13% and 2.5%－17%，respectively．The results showed that this method was suitable for the determination of PAHs and OPFRs in atmospheric particulate matter samples. |
| Key Words:high performance solvent extraction solid phase extraction gas chromatography－mass spectrometry polycyclic aromatic hydrocarbons organophosphorus flame retardants atmospheric particulate matters |
| 引用本文：张天琪，李圣增，张厚勇，齐安安，徐鹏，杨凌霄.高效溶剂萃取－固相萃取/气相色谱－质谱法测定大气颗粒物中多环芳烃和有机磷阻燃剂[J].分析测试学报,2022,41(11):1600-1606. |
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