Determination of 20 halogenated polycyclic aromatic hydrocarbons in gaseous and particulate samples of ambient air by gas chromatography-triple quadrupole mass spectrometry with accelerated solvent extraction and silica gel column purification
The contents of halogenated polycyclic aromatic hydrocarbons(HPAHs)in ambient air are usual-ly at the level of picogram(pg),and the interference of matrix is great,so it is difficult to determine their contents accurately.In this study,the accelerated solvent extraction(ASE)was conducted using n-hexane and dichloromethane(volume ratio of 1∶1)as the extracting solvent.The silica gel column was used for purification using n-hexane and dichloromethane(volume ratio of 3∶2)as the elution solvent.Phenan-threne-d10,chrysene-d12 and perylene-d12 were selected as the internal standard for quantification.The anal-ysis method for the simultaneous determination of 20 HPAHs in gaseous and particulate samples of ambi-ent air by gas chromatography-triple quadrupole mass spectrometry(GC-QQQ-MS/MS)was established.The experimental results showed that the calibration curves of 20 HPAHs in range of 0.1-20.0 pg/μL had good linear relationship with correlation coefficient of r＞0.995.The limit of detection was 0.05-0.4 pg/μL,and the limit of quantification was 0.1-1.5 pg/μL.The standard addition tests of two blanks with high and low concentration level were conducted.The results showed that the recoveries of 20 HPAHs at low concentration(0.4pg/μL)were between 75％and 113％,and the relative standard deviations(RSD,n=6)were between 0 and 15.6％.At high concentration(5.0 pg/μL),the recoveries of 20 HPAHs were between 82％and 97％,and the RSDs were between 1.8％and 5.8％.The testing results could meet the related re-quirements of spiked recovery and RSD for polycyclic aromatic hydrocarbons(PAHs)in HJ 646-2013.The proposed method was applied for the analysis of sample and sample with standard addition.The concentra-tion of 20 HPAHs detected in gaseous and particulate samples of ambient air ranged from undetected to 2.0 pg/μL.When the standard addition concentration was 3.0 pg/μL,the average recoveries of 20 HPAHs were between 80％and 107％,and the RSDs(n=6)were between 2.9％and 8.2％.
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万方数据
维普
