自组装固相萃取-气相色谱-质谱法测定大气细颗粒物中溴代多环芳烃类化合物  

Determination of Brominated Polycyclic Aromatic Hydrocarbons in Atmospheric Fine Particulate Matter by Self-assembled Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

作　　者：张宇 王椿 辛悦 徐建中[1] 王美 ZHANG Yu;WANG Chun;XIN Yue;XU Jian-Zhong;WANG Mei(College of Chemistry and Environmental Science,Hebei University,Baoding 071002,China)

机构地区：[1]河北大学化学与环境科学学院,保定071002

出　　处：《分析化学》2023年第10期1641-1650,共10页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(No.21906038);河北省高等学校科学技术研究项目(No.QN2021019)资助

摘　　要：基于气相色谱-质谱联用技术,建立了大气细颗粒物(PM2.5)中13种溴代多环芳烃(Br-PAHs)的定性和定量分析方法。大气样品以正己烷-二氯甲烷混合溶剂(1∶1,V/V)进行加速溶剂萃取,经自组装硅胶柱净化后,采用DB-5MS色谱柱(30 m×0.25 mm×0.25μm)分离,在电子轰击电离源下,以选择离子模式,采用外标法定量分析。在优化的分析条件下,13种Br-PAHs的仪器检出限为0.12~0.58 pg/m^(3),定量限为0.25~1.70 pg/m^(3)。本方法线性关系良好,相关系数为0.9950~0.9994,低、中、高3个浓度水平的加标回收率为68.9%~111.5%,相对标准偏差为1.4%~12.8%。将此方法应用于实际PM2.5中Br-PAHs的测定,结果表明,PM2.5样品中13种Br-PAHs的总浓度为21.20~214.80 pg/m^(3)。除9-溴蒽未检出外,其它12种化合物的检出率均高于58%。其中,9,10-二溴菲和1-溴蒽为主要污染物,浓度分别为0.30~64.20 pg/m^(3)和ND~95.40 pg/m^(3)。本方法前处理快速简单,一次处理即可完成13种Br-PAHs的分析检测,具有精确度高和重复性好等特点,并且气相色谱-单四极杆质谱仪应用广泛,便于相关技术的推广。Based on gas chromatography-mass spectrometry,a qualitative and quantitative method was developed for determination of 13 kinds of brominated polycyclic aromatic hydrocarbons(Br-PAHs)in fine particulate matter(PM2.5).The atmospheric samples were extracted with a mixture of hexane-dichloromethane(1∶1,V/V),purified by a self-assembled silica gel column,separated by a DB-5MS column(30 m×0.25 mm×0.25μm),and quantified by external standard method with selective ion mode under electron bombardment ionization source.Under optimized analytical conditions,the limits of detection and quantitation of 13 kinds of Br-PAHs were 0.12-0.58 pg/m^(3)and 0.25-1.7 pg/m^(3),respectively.The linear relationship of the method is good,and the correlation coefficient is 0.9950-0.9994.The recoveries were 68.9%-111.5%and the relative standard deviations at low,middle and high spiking levels were 1.4%-12.8%.The method was applied to determination of Br-PAHs in PM2.5 samples,and it was found that the total concentration of Br-PAHs in PM2.5 samples was 21.2-214.8 pg/m^(3),and the detection rates of the other 12 kinds of compounds were all higher than 58%except for the undetected 9-bromoanthracene.Among them,9,10-dibromophenanthrene and 1-bromoanthracene were the main pollutants with concentration ranges of 0.30-64.2 pg/m^(3)and ND-95.4 pg/m^(3),accounting for 1.3%-29.9%and 0-53.4%of the total concentrations of Br-PAHs.This method was fast and simple,and could complete the analysis and detection of 13 kinds of Br-PAHs in one processing.The quadrupole mass spectrometer was widely used,which was more cost saving than expensive high resolution mass spectrometry.

关 键 词：溴代多环芳烃 大气细颗粒物 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] X831[理学—化学]