摘要
建立了分散液液微萃取(DLLME)结合气相色谱串联质谱(GC-MS)测定土壤中痕量多环芳烃(PAHs)的新方法。采用QuEChERS(Quick、Easy、Cheap、Effective,Rugged和Safe)和DLLME对土壤中的15种PAHs进行了提取与富集,考察提取溶剂、净化剂用量、萃取溶剂种类及用量对提取效果的影响。结果表明,10 g土壤样品以20 mL V(甲醇)∶V(二氯甲烷)=1∶1混合溶剂为提取溶剂、150 mg W(PSA)∶W(C_(18))=4∶1吸附剂净化,2 mL上清液加100μL甲苯作为分散、萃取剂时最佳。所建方法在6~500μg/L范围内呈良好的线性关系,且R^(2)≥0.9995;检测限(LODs)和定量限(LOQs)分别为0.1~1.8、0.3~6.1μg/kg。在1、5、25μg/kg加标水平下,PAHs回收率为70.23%~108.52%,相对标准偏差(RSDs)为1.04%~11.63%。方法简便、快速、易于提取和富集,适用于包括澄迈县在内土壤中PAHs灵敏测定。
A new method for the determination of trace polycyclic aromatic hydrocarbons(PAHs)in soil by dispersive liquid-liquid microextraction(DLLME)combined with gas chromatography-tandem mass spectrometry(GC-MS)was established.Fifteen PAHs in soil were extracted and enriched by QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)and DLLME.The effects of extraction solvent,decontaminant dosage,type and dosage of extraction solvent on extraction efficiency were investigated.The 10 g soil samples were extracted with 20 mL V(methanol)∶V(dichloromethane)=1∶1 mixed solvent,purified with 150 mg W(PSA)∶W(C_(18))=4∶1 adsorbent.When 2 mL supernatant was added with 100μL toluene as dispersing and extracting agent,the effect was the optimal.There was the good linearity for the established method in the range of 6~500μg/L,and R^(2)≥0.9995;the detection limits(LODs)and quantitative limits(LOQs)were 0.1~1.8,0.3~6.1μg/kg,respectively.The recoveries of PAHs ranged from 70.23%to 108.52%and the relative standard deviations(RSDs)ranged from 1.04%to 11.63%at the level of 1,5 and 25μg/kg.The method is simple,rapid,easy to extract and enrich,it is suitable for sensitive determination of PAHs in soil including Chengmai County.
作者
王传咪
谭华东
武春媛
翟金玲
WANG Chuan-mi;TAN Hua-dong;WU Chun-yuan;ZHAI Jin-ling(College of Tropical Crops,Hainan University,Haikou 570228,China;Institute of Environment and Plant Protection,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China;National Danzhou Observation and Experiment Station for Agricultural Environment,Danzhou 571737,China)
出处
《化学试剂》
CAS
北大核心
2022年第5期755-761,共7页
Chemical Reagents
基金
农业农村部财政基金项目(NFZX-2019)
国家自然科学基金项目(42107501)
海南省自然科学基金项目(420QN316)
中国热带农业科学院环境与植物保护研究所基本业务费项目(hzsjy2021001)。
关键词
多环芳烃
QUECHERS
分散液液微萃取
气相色谱串联质谱
土壤
polycyclic aromatic hydrocarbons
QuEChERS
dispersive liquid-liquid microextraction
gas chromatography-mass spectrometry
soil
