同时测定PM_(2.5)中16种多环芳烃的超声提取-高效液相色谱法

Simultaneous determination of 16 kinds of polycyclic aromatic hydrocarbons in PM_(2.5) by ultrasonic extraction-high performance liquid chromatography

目的建立一种前处理过程简便、检测灵敏度高及重现性好,能同时测定空气中16种多环芳烃(PAHs)的检测方法。方法空气中的PAHs经玻璃纤维滤膜采集,乙腈-丙酮-正己烷混合溶剂提取,高效液相色谱测定。对不同的提取溶剂进行了比较,对超声提取的温度和时间进行了优化,获得了最佳的超声萃取条件;优化了梯度洗脱条件和荧光检测程序。结果采用Agilent PAH柱分离,柱温25℃,25 min即可完成对16种PAHs的测定。在最优条件下,PAHs在0.05~5μg/ml范围内线性关系良好,相关系数0.999 6~0.999 9。检出限范围0.03~0.59 ng/m^3。PAHs在0.2、1.0、5.0μg的加标回收率范围分别为77.5%~112.5%、70.9%~107.6%、67.9%~98.0%。平行测定7次RSD范围在0.63%~5.10%。结论该方法简便准确,检出限低,重复性好,灵敏度高,适用于空气中16种PAHs的测定。

[Objective]To establish a method for the simultaneous determination of 16 kinds of polycyclic aromatic hydrocarbons（PAHs）in air,with the features of simple pre-treatment,high sensitivity and good reproducibility.[Methods]PAHs in air were collected by glass fiber filter,extracted by acetonitrile-acetone-n-hexane and determined by high performance liquid chromatography（HPLC）. The experiment has compared the different extraction solvents,and optimized the temperature and time of ultrasonic extraction to obtain the best ultrasonic extraction conditions. Furthermore,the conditions of gradient elution and ultraviolet-fluorescence detection programs were optimized.[Results] PAHs could be separated well by Agilent PAH column within 25 minuts at 25 ℃. Under the optimal conditions,the linear relationship for PAHs was good within the range of 0.05-5 μg/ml,and the correlation coefficients were between 0.999 6 and 0.999 9. The detection limits were between 0.03 ng/m3 and 0.59 ng/m^3.The recovery rates of 0.2 μg,1.0 μg and 5.0 μg spiked sample PAHs were 77.5%-112.5%,70.9%-107.6% and 67.9%-98.0%,respectively. RSD was range from 0.63% to 5.10% by seven parallel determinations.[Conclusion] The method is easy and accurate with high sensitivity and good reproducibility,which is suitable for the detection of 16 kinds of PAHs in air.