高效液相色谱-二极管阵列检测器串联荧光检测法同时测定空气中的16种多环芳烃

Determination of 16 PAHs in air samples by high performance liquid chromatography with photo-diode array and fluorescence detector

目的通过研究色谱条件、提取条件、方法的检出下限、回收率、精密度等内容,确定利用高效液相色谱-二极管阵列检测器串联荧光检测法同时测定空气中16种多环芳烃含量的最佳测试方法。方法对滤膜采用10 ml乙腈超声提取1 h,涡旋振荡2 min,再超声提取1 h,涡旋振荡2 min,10 000 r/min离心5 min,取5 ml上清液氮气吹干,1 ml乙腈定容,过膜上样,高效液相色谱柱分离荧光测定,外标法定量。结果该方法对样品的检出限为0.10 ng/m3~0.26 ng/m3,相关系数>0.999。平均回收率在88.6%~103.2%,相对标准偏差在1.5%~4.3%。结论方法灵敏度高、操作简单、定量准确、测定浓度范围宽,是空气中16种多环芳烃含量检测的理想方法。

Objective To develop a best method based on high performance liquid chromatography with photo-diode array and fluorescence detector（ HPLC-PDA-FLD） for the determination of 16 polycyclic aromatic hydrocarbonds（ PAHs） in air samples by study of extraction conditions,chromatographic conditions,detection limit,recovery and precision. Methods The membrane samples were put in 10 ml acetonitrile and treated in ultrasonic extractor for 1 hour,then vibrated for 2 minutes,extracted in ultrasonic extractor for 1 hour again,vibrated for 2 minutes again and centrifuged at 10 000 r/min for 5 minutes. 5 ml supernatant fraction was blowed dry by nitrogen and dissolved by 1 ml acetonitrile. Then it was filtered and separated with HPLC,then determined by photo-diode array and fluorescence detector. Quantification was performed by external standard calibration.Results The detection limit was within 0. 10 ng/m3-0. 26 ng/m3. and correlation coefficient（ r） was above 0. 999,the average recovery rate was within 88. 6%-103. 2%. The relative standard deviation was within 1. 5%-4. 3%. Conclusion This method can be applied for the determination of 16 PAHs in air samples,which has high sensitivity,simple operation,accurate quantification and wide concentration range.