作者：谭华东1,2, 张汇杰1,3, 武春媛1,2
作者单位：1. 中国热带农业科学院环境与植物保护研究所, 海南 海口 571101;
2. 国家农业环境儋州观测实验站, 海南 儋州 571737;
3. 华中农业大学资源与环境学院, 湖北 武汉 430070
关键词：QuEChERS;气相色谱质谱;土壤;多环芳烃
摘要：
为实现土壤样品中典型持久性污染物的快速、灵敏及批量测定，通过基于改进微量-QuEChERS（μ-QuEChERS）技术结合超声辅助方法，且与气相色谱质谱联用（GC-MS）分析，建立土壤中16种多环芳烃（PAHs）快速测定方法。少量土壤（1.0 g）样品经过2.0 mL乙腈与二氯甲烷（V/V=1∶2）辅助15.0 min超声提取后，利用N-丙基乙二胺（PSA）和C18混合分散剂快速涡旋净化，离心、转换溶剂后进行GC-MS外标法测定。结果表明，在2~800 μg/L浓度范围内，16种PAHs呈现良好的线性关系，相关系数均在0.992 0以上，检测限（LOD，S/N=3）低于0.50 μg/kg。在8.0，20.0，100.0 μg/kg加标浓度下，16种PAHs的加标回收率在70.3%~109.1%（n=3）。该方法快速、简单、准确，需样量少、环境污染小，可为土壤中PAHs的快速筛查提供批量检测方法。
Rapid determination of 16 polycyclic aromatic hydrocarbons in soil by gas chromatography-tandem mass spectrometry coupled with micro-QuEChERS
TAN Huadong1,2, ZHANG Huijie1,3, WU Chunyuan1,2
1. Environment and Plant Protection Institute, Chinese Academy of Tropical Agricultural Sciences, Haikou 571101, China;
2. National Agricultural Experimental Station for Agricultural Environment, Danzhou 571737, China;
3. School of Resources and Environment, Central China Agricultural University, Wuhan 430070, China
Abstract: A new method was established to rapidly determine 16 polycyclic aromatic hydrocarbons (PAHs) in soil using gas chromatography-tandem mass spectrometry (GC-MS) coupled with micro-QuEChERS (μ-QuEChERS). The target compounds were extracted from 1.0 g of soil samples using 2 mL acetonitrile and dichloromethane (V/V=1:2) assisted with ultrasound for 15 min, and then were purified by the mixed dispersant (primary secondary amine (PSA) and C18). After centrifugation and conversion solvent, the supernatants were determined by GC-MS based on external standard method. The results showed that there were good linear relationships to 16 target compounds in the range of 2-800 μg/L. The correlation coefficients of the established method were above 0.992 with the limits of detections (LODs, S/N=3) below 0.50 μg/kg. At three spiked of 8.0, 20.0 and 100.0 μg/kg, the recoveries of 16 PAHs were 70.3%-109.1% (n=3). The method is fast, simple, accurate, sample-less and pollution-less, which can provide batch detection method for rapid screening of PAHs contamination in soils.
Keywords: QuEChERS;GC-MS;soil;polycyclic aromatic hydrocarbons
2020, 46(1):64-70 收稿日期: 2019-04-22;收到修改稿日期: 2019-06-08
基金项目: 海南省重大科技计划(ZDKJ2017002)；中国热带农业科学院基本科研业务费专项资金（1630042019020）；中国热带农业科学院环境与植物保护研究所项目结余经费自主选题专项（hzsjy2018003）
作者简介: 谭华东(1991-),男,湖南郴州市人,研究实习员,硕士,研究方向为有机污染的环境行为
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