作者：车凯¹, 郑宇超², 范辉³, 魏明磊³, 刘克成¹, 周慧波¹, 谌杨²

作者单位：1. 国网河北省电力有限公司电力科学研究院，河北 石家庄 050021;
2. 中油工程项目管理分公司廊坊中油朗威工程项目管理有限公司，河北 廊坊 065000;
3. 国网河北省电力有限公司，河北 石家庄 050021

关键词：超声波萃取;气相色谱-质谱法;土壤;多环芳烃;多氯联苯

摘要：

建立超声波萃取结合气相色谱-质谱法(GC-MS)同时分析土壤中16种多环芳烃(PAHs)和18种多氯联苯(PCBs)的方法，并比较不同萃取方式、超声萃取时间和萃取次数等对加标回收率的影响。得到最佳检测方法为10.0 g样品用20 mL的正己烷和丙酮混合液(体积比1∶1)超声波萃取15 min，萃取4次，萃取液经过浓缩、净化后，采用GC-MS进行分析。结果表明：16种PAHs和18种PCBs的标准曲线线性关系良好，方法线性相关系数>0.999，方法检出限为0.9~2.5 μg/kg。空白石英砂平均加标回收率为69.7%~123.4%，相对标准偏差在1.1%~9.1%之间，土壤样品平均加标回收率为64.6%~134.1%，替代物回收率在72.1%~119.6%之间。相对标准偏差为5.1%~15.7%。该方法实用性强，检测周期短，回收率和检出限均能满足样品分析质量控制要求，适合土壤中PAHs和PCBs的同时检测。

Development of ultrasonic extraction method for simultaneous determination of PAHs and PCBs in soil combine GC-MS
CHE Kai¹, ZHENG Yuchao², FAN Hui³, WEI Minglei³, LIU Kecheng¹, ZHOU Huibo¹, CHEN Yang²
1. State Grid Hebei Electric Power Research Institute, Shijiazhuang 050021, China;
2. CNPC China Petroleum LONGWAY Engineering Project Management Co., Ltd., Langfang 065000, China;
3. State Grid Hebei Electric Power Company, Shijiazhuang 050021, China
Abstract: A method for simultaneous analysis of 16 polycyclic aromatic hydrocarbons (PAHs) and 18 polychlorinated biphenyls (PCBs) in soil by ultrasonic extraction combined with gas chromatography-mass spectrometry (GC-MS) was established, and the effects of different extraction methods, ultrasonic extraction time and extraction times on standard recovery were compared.The best detection method was the ultrasonic extraction of 10.0 g sample with 20 mL mixture of n-hexane and acetone (volume ratio: 1∶1) for 15 min and extraction for 4 times. After the extraction solution was concentrated and purified, GC-MS was used for analysis. The results showed that the standard curve of 16 PAHs and 18 PCBs had good linear relationship. The linear correlation coefficient of the method was greater than 0.999, and the detection limit of the method was 0.9-2.5 μg/kg. The average standard recovery of blank quartz sand is 69.7%-123.4%, the relative standard deviation is 1.1%-9.1%, the average standard recovery of soil sample is 64.6%-134.1%, the recovery of substitute is 72.1%-119.6%. The relative standard deviation is 5.1%-15.7%. This method has strong practicability, short detection period, and the recovery rate and detection limit can meet the quality control requirements of sample analysis. It is suitable for simultaneous detection of PAHs and PCBs in soil.
Keywords: ultrasonic extraction;GC-MS;soil;PAHs;PCBs
2021, 47(5):68-75  收稿日期: 2020-12-10;收到修改稿日期: 2021-02-05
基金项目: 国家电网公司科技项目(5204DY19000A)
作者简介: 车凯(1985-),男,河北石家庄市人,高级工程师,硕士,主要从事电力环保工作的相关研究
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