基质固相分散-稳定同位素稀释-气相色谱-质谱联用测定土壤中多环芳烃  

Determination of polycyclic aromatic hydrocarbons in soil sample using matrix solid phase sispersion-stable isotope dilution technique-gas chromatography mass spectrometry

作　　者：张永涛[1] 张莉[1] 李义 李晓亚[1] 桂建业[1] 赵国兴[1] 

机构地区：[1]中国地质科学院水文地质环境地质研究所,河北正定050803 [2]河北省环境地质勘查院,河北石家庄050021

出　　处：《中国卫生检验杂志》2017年第7期923-925,930,共4页Chinese Journal of Health Laboratory Technology

基　　金：地质调查工作项目(1212011120379);中国地质科学院基本科研项目(SK201203)

摘　　要：目的采用基质固相分散前处理技术及稳定同位素稀释技术,建立气相色谱-质谱联用测定土壤中多环芳烃的方法。方法样品采用C_(18)键合硅胶作为固相分散剂,利用氘代化合物作为同位素稀释剂,采用二氯甲烷-丙酮进行洗脱。结果 10次多环芳烃与同位素稀释剂面积比值的相对标准偏差(RSD)均<2.5%,验证了氘代化合物和目标物相似的物理化学性质及色谱行为的一致性,证实了在本实验样品前处理过程中同位素分馏现象不明显。采用同位素稀释法定量,加标回收率为88.5%~105.8%,精密度为0.89%~3.06%。结论该方法样品前处理过程较为简单,同位素稀释法校正了前处理过程中的损失,定量更加准确可靠,可以满足检测土壤中多环芳烃的要求。Objective A method for the determination of polycyclic aromatic hydrocarbons（PAHs） in soil by gas chromatography mass spectrometry was developed based on matrix solid phase dispersion pretreatment technology and stable isotope dilution technique.Methods The sample adopted silica with bonded C_（18） as solid supports,deuterium compound was used as dichloromethane-acetone,and dichloromethane acetone was used to elute.Results All the relative standard deviation（RSD） of 10 times of area ratio of polycyclic aromatic hydrocarbons and isotope were less than 2.5%,which verified the consistence of physicochemical properties and chromatographic behavior between deuterium compound and target compounds,and confirmed that the isotope fractionation was not obvious during the sample pretreatment in this experiment.When using isotope dilution method,the accuracy and recovery rate was within 88.5%-105.8%,precision was within 0.89%-3.06%.Conclusion The sample pretreatment of this method is relative easy,and the isotope dilution method corrected the loss during the pretreatment process.Its means quantitative result is more precise and reliable,and can meet the requirement of detection polycyclic aromatic hydrocarbons in soil.

关 键 词：基质固相分散 同位素稀释 多环芳烃 气相色谱质谱仪 

分 类 号：O657.63[理学—分析化学]