磷化工业园区表层土壤16种多环芳烃检测方法建立  

Establishment of detection methods for 16 polycyclic aromatic hydrocarbons in surface soil of a phosphating industrial park

作　　者：李国文 胡柠檬 尤买艳 刘宇 刘淑娟 Li Guo-wen;Hu Ning-meng;YOU Mai-yan;LIU Yu;LIU Shu-juan(Ecological and Environmental Monitoring Station of DEEY in Yuxi,Yuxi 653100,China;Fuxian Lake Station of Plateau Lake in Yunnan(Wetland),Yuxi 653100,China;College of Chemistry,Biology,and Environment,Yuxi Normal University,Yuxi 653100,China;College of Resources,Environment and Chemistry,Chuxiong Normal University,Chuxiong 675000,China)

机构地区：[1]云南省生态环境厅驻玉溪市生态环境监测站,云南玉溪c653100 [2]云南抚仙湖高原湖泊站(湿地),云南玉溪653100 [3]玉溪师范学院化学生物与环境学院,云南玉溪653100 [4]楚雄师范学院资源环境与化学学院,云南楚雄675000

出　　处：《化学研究与应用》2025年第4期1026-1033,共8页Chemical Research and Application

基　　金：云南省地方高校联合专项-青年项目(202101BA070001-263)资助;云南省教育厅科学研究基金项目(2022JO829)资助,云南省教育厅科学研究基金项目(2024J0888)资助;云南省基础研究专项-青年项目(202301AU070019)资助。

摘　　要：为实现磷化工业园区表层土壤多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的检测,建立了加速溶剂萃取结合气相色谱-质谱(GC-MS)测定16种PAHs残留的分析方法。并对仪器关键参数及样品前处理步骤进行了优化,采用加速溶剂对样品进行预处理,选择离子监测(selective ion monitoring,SIM)模式检测,HP-5MS色谱柱分离,氘代内标法定量,16种PAHs可在20.0 min内完成色谱分离分析。实验结果表明,在最优提取条件下,16种PAHs线性(10~1000μg·L^(-1))关系良好,平均相对响应因子(RRF)的相对标准偏差(RSD)小于7.4%,方法检出限为0.1~0.4μg·kg^(-1),定量下限为0.4~1.6μg·kg^(-1)。在空白样品添加3个不同质量比(2.5、10、50μg·kg^(-1))水平下,测得16种PAHs的平均回收率为65.7~93.4%、相对标准偏差(n=6)为0.5~9.1%。研究建立的方法具有简便快捷、回收率高、选择性强等优点,适合磷化工园区表层土壤中16种PAHs残留检测。To achieve the detection of polycyclic aromatic hydrocarbons(PAHs)in the surface soil of phosphating industrial park,an analytical method for the determination of 16 PAHs residues by accelerated solvent extraction combined with gas chromatographymass spectrometry was established.To achieve the purpose,this method optimizes the key parameters of the instrument and the key steps of sample pre-processing.Specifically,accelerated solvent extraction was used for sample pretreatment,selective ion monitoring(SIM)mode was used for detection,HP-5 MS chromatographic column was used for separation,and deuterated internal standard method was used for quantification.Finally,16 PAHs could be separated and analyzed within 20 min.The findings revealed the calibration curves showed good linearities for 16 PAHs under the optimal extraction conditions,and the relative deviation of the response factor being less than 7.4%in the range of 10 to 1000μg·L^(-1).Whereas the limits of detection and limits of quantification for 16 PAHs under study should be within the range of 0.1 to 0.4μg·kg^(-1)and 0.4 to 1.6μg·kg^(-1),respectively.And,next,The average recoveries of 16 PAHs at three(2.5,10,and 50μg·kg^(-1))levels of blank sample addition ranged from 65.7%to 93.4%,with the relative standard deviations(RSDs,n=6)of 0.5%to 9.1%.Therefore,the evaluation results we have gained can prove can prove that the method we have developed enjoys the privilege of simple and rapid,high recovery rate and high selectivity.And,so,it can be adopted as a novel method to determine 16 PAHs in the surface soil of phosphating industrial park.

关 键 词：多环芳烃(PAHs) 土壤 磷化工业园区 加速溶剂萃取 气相色谱-质谱(GC-MS) 

分 类 号：O657.63[理学—分析化学]