固相萃取柱净化-液相色谱法测定大气中多环芳烃

DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN AEROSOLS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH CLEAN-UP BY SOLID-PHASE EXTRACTION COLUMN

建立以乙腈-水为流动相,高效液相色谱法测定大气颗粒物中16种优控多环芳烃化合物的方法.用玻璃纤维滤膜采集大气颗粒物,以二氯甲烷为溶剂,超声波提取样品,提取液过滤经溶剂转换后在C18硅胶柱上分离净化,洗脱液经氩气吹干浓缩后用乙腈定容,用乙腈-水作流动相进行高效液相色谱梯度洗脱分离,荧光检测器变波长程序检测.通过实验优化了16种多环芳烃化合物的分离和测定条件.16种PAH检测限为0.023～0.45 μg/L,日内(n=5)和日间(n=5)相对标准偏差分别为小于1.20%和小于2.3%.该法具有快速、灵敏、准确、重现性好的优点,适合于大气中痕量多环芳烃的测定.

Sixteen priority polycyclic aromatic hydrocarbons (PAHs) in aerosols were determined with a clean-up procedure by solid phase extraction and HPLC using acetonitrile/water as mobile phase. The analytical procedure includes collecting aerosols on glass fiber filter, ultrasonic extraction with dichloromethane and clean-up by solid-phase extraction, followed by separation and quantitation with HPLC using gradient elution and fluorescence programmed multiple wavelength shift detection. The separation and determination parameters were optimized. The detection limits of 16 PAHs are 0. 023-0. 45 μg/L. The study offers a rapid and accurate method for determination of the trace PAHs in aerosols.