加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤中16种多环芳烃  

Analysis of 16 polycyclic aromatic hydrocarbons in soil with accelerated solvent extraction, rotary evaporation for obtain a constant volume and high performance liquid chromatography

作　　者：陶鑫[1] 全洗强 俞建国[1] 杜文越[1] 秦愫妮[1] TAO Xin;QUAN Xiqiang;YU Jianguo;DU Wenyue;QIN Suni(Institute of Karst Geology,CAGS/Key Laboratory of Karst Dynamics,MNR&GZAR,Guilin,541004,China)

机构地区：[1]中国地质科学院岩溶地质研究所自然资源部/广西壮族自治区岩溶动力学重点实验室

出　　处：《环境化学》2019年第12期2797-2807,共11页Environmental Chemistry

基　　金：中国地质科学院岩溶地质研究所科研业务费项目(2017027)资助~~

摘　　要：建立了加速溶剂萃取-旋蒸定容-高效液相色谱法检测土壤样品中16种多环芳烃(PAHs)的方法.旋蒸定容有效减少了污染物的引入,特别是萘、菲.研究了影响PAHs回收率的主要因素.优化后的条件为:萃取温度110℃,静态萃取时间3 min,冲洗量30%,氮气吹扫时间30 s,正己烷/丙酮(体积比2∶1)为萃取液,1次静态萃取循环,弗罗里硅土柱为固相萃取小柱,正己烷/二氯甲烷(体积比7∶3)为淋洗液,淋洗液体积10 mL.在20—200 mg·L^-1范围内,各目标物线性关系(R2)为0.9994—1.目标物的检出限和定量限分别为0.08—2.50 mg·kg^-1和0.25—8.33 mg·kg^-1.在优化的实验条件下,加标水平为25 mg·kg^-1和100 mg·kg^-1时,目标物平均加标回收率分别为73.9%—105%、79.0%—110%,相对标准偏差(n=7)均小于10%.土壤PAHs QC样品的检测中,各目标物检测值均在参考值范围内;土壤PAHs QC样品加标回收率为63.4%—94.8%,适合实际土壤样品中多环芳烃的检测.A method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs)in soil by high performance liquid chromatography was proposed based on accelerated solvent extraction and rotary evaporation to obtain a constant volume.The introduction of pollutants,especially for naphthalene and phenanthrene,could be effectively reduced by rotary evaporation to obtain a constant volume.The main factors affecting the recoveries of PAHs were investigated.Optimized conditions are:110℃extraction temperature,three minutes static extraction,30%rinse volume,30 s nitrogen purge,a mixture of hexane and acetone(2∶1,V/V)for extraction solvent,one static extraction cycle,florisil was used as SPE column,mixture of hexane and dichloromethane(7∶3,V/V)as eluent,and 10 mL eluent volume.The correlation coefficients(R2)for PAHs were between 0.9994 and 1 in the range of 20—200 mg·L^-1.The limits of detection and quantitation of PAHs were 0.08—2.50 mg·kg^-1 and 0.25—8.33 mg·kg^-1,respectively.Under the optimized experimental conditions,the recoveries of PAHs,with 25 mg·kg^-1 and 100 mg·kg^-1 standard addition,were in the range of 73.9%—105%and 79.0%—110%,respectively,while the relative standard deviations(n=7)was less than 10%.In the detection of PAHs in soil QC sample,the concentrations of all the values of target analytes were within the reference value ranges and the recoveries were 63.4%—94.8%.Therefore,the present protocol is satisfactory for the detection of PAHs in actual soil samples.

关 键 词：加速溶剂萃取 旋蒸定容 高效液相色谱 土壤 多环芳烃( PAHs) 

分 类 号：X833[环境科学与工程—环境工程]