Helmholtz Zentrum München, German Research Center for Environmental Health, Institute of Ecological Chemistry, Ingolstädter Landstr. 1, 85764 Neuherberg, Germany.
J Chromatogr A. 2010 Mar 5;1217(10):1636-46. doi: 10.1016/j.chroma.2010.01.029. Epub 2010 Jan 18.
The development, optimization and validation of a liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (LC-APPI/MS/MS) method for the determination of 15 azaarenes (4-azafluorene, benzo[h] and -[f]quinoline, phenanthridine, acridine, 1-azafluoranthene, 4-azapyrene, benz[a]- and -[c]acridine, -10-azabenzo[a]pyrene, 7,9- and 7,10-dimethylbenz[c]acridine, dibenz[a,j]-, -[c,h] and [a,i]acridine) in airborne particulate matter is described. Each compound was detected and quantified operating in multiple reaction monitoring mode. Extraction of azaarenes was achieved using accelerated solvent extraction (ASE) with dichlormethane/methanol (50/50, v/v). After extraction, no additional clean-up procedure like solid phase or liquid/liquid extraction was necessary. Limits of quantification (S/Nx10) ranged from 0.2 pg/microl to 1.4 pg/microl, matrix dependent recoveries were between 57% and 94%, with relative standard deviations from 8% to 17%. Applicability of the method was demonstrated analyzing 10 samples of particulate matter (PM(2.5)) collected in winter 2008. In all samples dimethylbenz[c]acridines as well as dibenzacridines were below the limit of quantification, concentration of the remaining analytes were in the range from 0.002 ng/m(3) to 0.356 ng/m(3).
建立了测定大气颗粒物中 15 种氮杂芳烃(4-氮芴、苯并[h]和苯并[f]喹啉、菲啶、吖啶、1-氮芴、4-氮菲、苯并[a]和苯并[c]吖啶、-10-氮杂苯并[a]芘、7,9-和 7,10-二甲基苯并[c]吖啶、二苯并[a,j]、-[c,h]和[a,i]吖啶)的液相色谱-大气压光电离串联质谱法(LC-APPI/MS/MS)。每种化合物均采用多反应监测模式进行检测和定量。采用二氯甲烷/甲醇(50/50,v/v)加速溶剂萃取(ASE)提取氮杂芳烃。萃取后,无需固相萃取或液/液萃取等进一步的净化程序。定量限(S/Nx10)范围为 0.2 pg/µL 至 1.4 pg/µL,基质相关回收率在 57%至 94%之间,相对标准偏差为 8%至 17%。该方法应用于 2008 年冬季采集的 10 个大气颗粒物(PM(2.5))样品的分析。在所有样品中,二甲基苯并[c]吖啶和二苯并吖啶均低于定量限,其余分析物的浓度范围为 0.002 ng/m(3)至 0.356 ng/m(3)。