PM_(2.5)中16种多环芳烃的高效液相色谱测定法

Determination of 16 polycyclic aromatic hydrocarbons in PM_(2.5) by HPLC

目的建立高效液相色谱-紫外-荧光串联测定PM2.5中16种多环芳烃(PAHs)的方法。方法样品以2.5 ml乙腈水浴超声提取60 min,取萃取液过滤;应用高效液相色谱仪,乙腈-水梯度洗脱,经Athena多环芳烃(PAHs)专用柱分离,紫外串联荧光检测器检测,以保留时间定性,外标法峰面积定量。结果 16种PAHs在0.02~2.0μg/ml范围内呈现良好的线性关系,相关系数均大于0.999,检出限在0.03~0.50 ng/m^3之间,平均回收率在93.6%~109.0%之间,相对标准偏差均小于5.5%。对标准品溶液的稳定性考察发现,16种PAHs标准使用液(2.0μg/ml)在避光-20℃条件下,在4个月内稳定性较好。结论该方法具有分析时间快、溶剂消耗少的优点。

[Objective]To develop a method for determination of 16 Polycyclic Aromatic Hydrocarbons（PAHs）in PM_（2.5）by high performance liquid chromatography（HPLC）with ultraviolet and fluorescence detcetion.[Methods]The samples were extracted by2.5 ml acetonitrile in an ultrasonic bath for 60 minutes,and the extraction liquid was filtrated. The extraction was treated with acetonitrile and water as mobile phase of gradient elution,and separated by Athena（PAHs）column. HPLC/UV-FLD detector was used to detect the concentrations of PAHs,which were qualitatively determined by retention time and quantitatively determined by peak area of external standard calibration. [Results]The method had a good linear relationship in the concentration range of0.02- 2.0 μg/ml for 16 PAHs,and the relative coefficients were higher than 0.999. The range of detection limits were within0.03-0.50 ng/m^3,the average recovery rates were between 93.6% and 109.0%,and the relative standard deviations were below5.5%. The stability test showed that the standard solutions of 16 PAHs were able to keep at least 4 months away from light at-20 ℃.[Conclusion]The method has distinct advantages in rapid analysis and low solvent consumption.