超高效液相色谱法测定大气细颗粒物中16种多环芳烃

Determination of 16 polycyclic aromatic hydrocarbons in atmospheric fine particulate matter by ultra performance liquid chromatography

目的建立采用超高效液相色谱(UPLC)-二极管阵列检测器(PAD)-荧光检测器(FLD)串联同时快速检测大气细颗粒物(PM2.5)中16种多环芳烃的方法。方法大气细颗粒物中多环芳烃经玻璃纤维滤膜富集后用乙腈提取,使用PAH色谱柱分离,以甲醇、乙腈和水梯度洗脱,二极管阵列检测器检测苊烯,荧光检测器检测其余15种多环芳烃,外标法定量。结果 16种多环芳烃在15 min内完全分离。在0.01μg/ml^0.5μg/ml,峰面积和质量浓度的线性关系良好(r>0.999 9)。以低、中、高3种浓度(0.2μg、1.0μg、5.0μg)作为不同的添加水平,平均加标回收率为90.0%~111.8%。方法相对标准偏差为0.12%~0.87%(n=8),检出限为0.004 ng/m^3~0.19 ng/m^3;定量限为0.05 ng/m^3~0.76 ng/m^3。结论该方法简便、快速、灵敏、准确,能满足大气细颗粒物中16种多环芳烃的检测要求。

Objective To establish a method of ultra high performance liquid chromatography（ UPLC） coupled with photodiode array detector（ PAD） and fluorescence detector（ FLD） for analyzing 16 kinds of polycyclic aromatic hydrocarbons in atmospheric fine particulate matter（ PM2. 5）. Methods Polycyclic aromatic hydrocarbons（ PAHs） in atmospheric fine particulate matter were extracted by glass fiber membrane and extracted with acetonitrile,separated by PAH column,and gradiently eluted by methanol,acetonitrile and water. Acenaphthylene was determined by photodiode array detector,and the other 15 kinds of polycyclic aromatic hydrocarbons were determined by fluorescence detector using external standard method. Results 16 kinds of PAHs were completely separated within 15 minutes. In 0. 01 μg/ml-0. 5 μg/ml,the linear relationship between peak area and mass concentration was good（ r〉 0. 999 9）. At low,medium and high different addition levels（ 0. 2 μg,1. 0 μg and5. 0 μg）,the average recoveries was within 90. 0%-111. 8%,the relative standard deviation was within 0. 12%-0. 87%（ n = 8）,the detection limit was within 0. 004 ng/m^3-0. 19 ng/m^3,the limit of quantification was within 0. 05 ng/m^3-0. 76 ng/m^3. Conclusion This method is simple,rapid,accurate and sensitive,and it can be used for determining 16 kinds of PAHs in atmospheric fine particulate matter.