超声提取-在线固相萃取浓缩/液相色谱法测定大气颗粒物中超痕量多环芳烃  

Determination on Ultra-trace of Polycyclic Aromatic Hydrocarbons in Atmospheric Particulate Matters by Liquid Chromatography Coupled with Ultrasonic Extraction and Online Solid Phase Extraction Concentration

作　　者：黄肇章 王超[1] 齐炜红 陈烨[1] 袁懋[1] HUANG Zhao-zhang;WANG Chao;QI Wei-hong;CHEN Ye;YUAN Mao(China National Environmental Monitoring Centre,Beijing 100012,China;Guangzhou Environmental Monitoring Centre,Guangzhou 510091,China;Handan Environmental Monitoring Centre,Handan 056000,China)

机构地区：[1]中国环境监测总站,北京100012 [2]广州市环境监测中心站,广东广州510091 [3]邯郸市环境监测站,河北邯郸056000

出　　处：《分析测试学报》2021年第7期1025-1030,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2016YFC0208506)。

摘　　要：建立了超声提取-在线固相萃取浓缩/液相色谱测定大气颗粒物中15种多环芳烃(PAHs)的方法。通过优化仪器分析条件、样品提取和制备条件以及消除离子干扰等,确定了最佳的实验条件。切取1.4 cm^(2)颗粒物滤膜样品,使用2 mL乙腈超声提取10 min。提取液经高速离心去除悬浮颗粒物后,配制为25%(体积分数)乙腈水溶液。取2 mL提取液,经Acclaim Polar AdvantageⅡC_(18)固相萃取柱(50 mm×4.6 mm,3μm)富集和净化,采用Hypersil Green PAH色谱柱(150 mm×3 mm,3μm)和0.05 mol/L乙酸铵溶液-乙腈流动相分离15种PAHs,通过荧光检测器进行检测。15种PAHs在一定的质量浓度范围内线性良好,相关系数均大于0.992;按照采样大气体积为23 m^(3),采集的滤膜面积12 cm^(2)计算,方法检出限为0.03×10^(-3)~33.27×10^(-3)ng/m^(3),其中苯并[a]芘的检出限为0.67×10^(-3)ng/m^(3);在低、高浓度下的加标回收率分别为91.4%~126%和103%~123%,相对标准偏差(RSD,n=6)分别为4.4%~10%和5.2%~12%。实际样品分析结果显示,该方法所需样品量少、灵敏度高、操作简便,可满足大气颗粒物中PAHs的超痕量分析要求。A liquid chromatography(LC)with ultrasonic extraction and online solid phase extraction(online SPE)concentration was developed for the determination of 15 polycyclic aromatic hydrocarbons(PAHs)in atmospheric particulate matters.Through the optimization of instrument analysis,sample extraction and preparation,and elimination of ion interference,the best experimental conditions were obtained.A slice of 1.4 cm^(2) was cut from a particulate filter membrane sample,and extracted with 2 mL acetonitrile by ultrasonic extration for 10 min.The extract was high-speedily centrifugated to remove the suspended particles,then prepared as an solution containing 25%(by volume)acetonitrile.2 mL of the prepared solution was directly injected into the online SPE/LC.Online purification and enrichment of the samples were carried out on an Acclaim Polar AdvantageⅡC_(18) SPE column(50 mm×4.6 mm,3μm).15 PAHs were separated on a Hypersil Green PAH column(150 mm×3 mm,3μm)with 0.05 mol/L ammonium acetate solution-acetonitrile as mobile phase,and detected by fluorescent detector.The linear correlation coefficients of the 15 PAHs were greater than 0.992.Calculated by air volume of 23 m^(3) and filter membrane area of 12 cm^(2),the limits of detection(LOD)of the method were in the range of 0.03×10^(-3)-33.27×10^(-3) ng/m^(3),in which the LOD for benzo(a)pyrene(B(a)P)was 0.67×10^(-3) ng/m^(3).The recoveries for 15 PAHs at two spiked levels of 40 ng/L and 200 ng/L were in the ranges of 91.4%-126%and 103%-123%,with relative standard deviations(RSD,n=6)of 4.4%-10%and 5.2%-12%,respectively.The method is simple,sensitive and low sample consumptive(1.4 cm^(2)),and could meet the requirements for analysis of ultra-trace PAHs in atmospheric particulate matters.

关 键 词：大气颗粒物 多环芳烃 液相色谱 超声提取 在线固相萃取 荧光检测 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]