超高效液相色谱法测定大气PM_(2.5)中16种多环芳烃

Determination of polycyclic aromatic hydrocarbons in PM_(2.5) by ultrasensitive performance liquid chromatography

[目的]建立检测大气细颗粒物(PM_(2.5))中16种多环芳烃的超高效液相色谱法。[方法]滤膜采用乙腈超声提取、浓缩后,以乙腈和水为流动相进行梯度洗脱,在PAH C18柱上分离,对样品前处理和色谱条件进行优化,用超高效液相色谱仪、二极管阵列检测器和荧光检测器进行测定。[结果]16种多环芳烃在12 min内得到了良好的分离,在0.01~0.50μg/mL范围内线性关系良好,检出限为0.003~0.036 ng/m^3,测定下限为0.010~0.119 ng/m^3;0.02、0.05、0.20μg三个加标水平下的平均回收率为68.5%~100.6%,相对标准偏差(n=7)在2.0%~7.3%之间。[结论]该法操作简便,具有分离时间短、分离效果好、灵敏度高的特点,适于大气PM_(2.5)样品中多环芳烃的测定。

Objective To develop a method for the determination of polycyclic aromatic hydrocarbons（PAHs） in atmospheric fine particulate matters（PM_（2.5）） by ultrasensitive performance liquid chromatography. Methods Samples were extracted and enriched with acetonitrile by ultrasonic wave. Then acetonitrile and water were used as mobile phase for gradient elution, and separation was conducted on a PAH C18 column. Sample preparation and chromatographic conditions were optimized. Ultrasensitive performance liquid chromatography, photodiode array detector, and fluorescence detector were used to detect PAHs. Results Sixteen PAHs were separated in 12 min, showing a good linearity in the range of 0.01-0.50 μg/m L. The limits of detection for the PAHs were 0.003-0.036 ng/m^3, and the limits of quantification were 0.010-0.119 ng/m^3. The average recoveries of 16 PAHs at 0.02, 0.05, and 0.20 μg spiked levels were 68.5%-100.6%, with relative standard deviations of 2.0%-7.3%（n=7）. Conclusion The method developed is simple, rapid, efficient, and sensitive; therefore, it is suitable for determination of PAHs in PM_（2.5）.