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
NIU Shaomin1,2, ZHANG Xin1,2, TIAN Weihua1,2, LI Fei1,2, WANG Ting1,2, XING Yan*1,2
1. Shaanxi Province Environmental Monitoring Center,Xi'an 710000,China; 2. Shaanxi Key Laboratory for Environmental Monitoring and Forewarning of Trace Pollutants,Xi'an 710000,China
Abstract：The contents of halogenated polycyclic aromatic hydrocarbons(HPAHs) in ambient air are usually 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.Phenanthrene-d10,chrysene-d12 and perylene-d12 were selected as the internal standard for quantification.The analysis method for the simultaneous determination of 20 HPAHs in gaseous and particulate samples of ambient 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 (0.4 pg/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 requirements 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 concentration 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%.
牛少敏, 张鑫, 田渭花, 李飞, 王婷, 杏艳. 加速溶剂萃取-硅胶柱净化-气相色谱-三重四极杆质谱法测定环境空气气态和颗粒态样品中20种卤代多环芳烃[J]. 冶金分析, 2024, 44(1): 35-43.
NIU Shaomin, ZHANG Xin, TIAN Weihua, LI Fei, WANG Ting, XING Yan. 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. , 2024, 44(1): 35-43.
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