摘要
建立了土壤中5种氯代多环芳烃和15种多环芳烃的超分子溶剂微萃取高效液相色谱荧光检测分析方法.探讨了萃取剂的组成、用量、涡旋振荡时间等因素对萃取效率的影响.优化后的实验条件为:以3 mL 1-辛醇、8 mL四氢呋喃和29 mL水混合制备超分子溶剂;400μL超分子溶剂加入200 mg样品中,斡旋震荡2 min,离心后上清液过0.22μm滤膜,目标化合物经多环芳烃专用柱(SUPELCOSILTMLC-PAH,150 mm×4.6 mm,5μm)乙腈-水梯度分离后荧光检测,外标法定量.结果显示,20种目标化合物在线性范围内呈现良好的线性关系,相关系数均大于0.999;目标化合物的基质加标回收率为76.5%—105.3%,相对标准偏差为0.2%—8.5%,方法的检出限(LOD,S/N=3)为0.07—2.3μg·kg^(−1),定量限(LOQ,S/N=10)为0.2—7.0μg·kg^(−1).该方法简便快速,样品处理过程不超过15 min,而且成本低廉,环境友好,可用于土壤中氯代多环芳烃和多环芳烃的快速分析检测.
An analytical method for determination of five kinds of chlorinated polycyclic aromatic hydrocarbons and fifteen kinds of polycyclic aromatic hydrocarbons in soil was developed using supramolecular solvent-based microextraction(SSBME)followed by high performance liquid chromatography coupled with fluorescence detection.The effects of the composition and amount of supramolecular solvent(SUPRAS)and vortex time on the extraction efficiency were systemically investigated.The supramolecular solvent was produced using 3 mL 1-octanol and 8 mL tetrahydrofuran and 29 mL water.200 mg of dried soil samples were effectively extracted with 400μL SUPRAS after vortexing for 2 min.After the centrifugation the supernatant was filtered by 0.22μm film and the extracts was analyzed via liquid chromatography-fluorescence detection.Neither evaporation nor further clean-up steps for the extracts were needed.The overall sample treatment took approximately 15 min and multiple samples can be processed simultaneously.The separation of the target compounds was achieved on a SUPELCOSILTMLC-PAH column(150 mm×4.6 mm,5μm)with acetonitrile-water as mobile phase using gradient elution.Quantitative determination was achieved by external standard method.The correlation coefficients(r)were greater than 0.999 in the linear ranges of 20 target compounds.The average recoveries of target compounds were 76.5%—105.3%and the corresponding relative standard deviations(RSD,n=3)were 0.2%—8.5%.The limits of detection(LOD,S/N=3)and limits of quantification(LOQ,S/N=10)were in the range of 0.07—2.3μg·kg^(−1) and 0.2—7.0μg·kg^(−1),respectively.The method is simple,rapid,cheap and environmentally friendly.It can be applied for the rapid determination of chlorinated polycyclic aromatic hydrocarbons and polycyclic aromatic hydrocarbons in soil samples.
作者
熊力
王金成
陈吉平
XIONG Li;WANG Jincheng;CHEN Jiping(Dalian Polytechnic University,Dalian,116034,China;Dalian Institute of Chemical Physics,The Chinese Academy of Sciences,Dalian,116023,China)
出处
《环境化学》
CAS
CSCD
北大核心
2022年第10期3159-3166,共8页
Environmental Chemistry
关键词
氯代多环芳烃
多环芳烃
超分子溶剂微萃取
高效液相色谱
土壤
chlorinated polycyclic aromatic hydrocarbons
polycyclic aromatic hydrocarbons
supramolecular solvent microextraction
high performance liquid chromatography
soil
