分子印迹固相萃取-气相色谱/质谱联用法测定污泥中多环芳烃

Determination of polycyclic aromatic hydrocarbons in sludge by molecular imprinting solid phase extraction and gas chromatography / mass spectrometry

本研究建立了检测污泥中16种多环芳烃(PAHs)的气相色谱-质谱测定方法,对该介质中16种多环芳烃(PAHs)的提取、净化和色谱质谱条件进行了优化.采用100 m L正己烷∶丙酮(V∶V,50∶50)混合溶剂索式提取样品中的待测组分,经分子印迹固相萃取柱(MIPs/SPE)净化,内标法定量.结果表明,分子印迹固相萃取柱(MIPs/SPE)对PAHs单体专一吸附效果显著,对中环、高环PAHs的吸附明显,并且基质效应减弱.16种多环芳烃的线性范围为10—5000 ng·m L^(-1),相关系数(R2)不低于0.9978,加标水平为50、250、500 ng·m L^(-1)时,基质平均加标回收率分别为60%—105%,58%—121%和63%—115%,相对标准偏差(RSDs,n=6)为3.8%—9.4%.该方法快速、准确、灵敏度高、重现性好.

A GC-MS method was developed and validated for the determination of sixteen PAHs in sludge. The PAHs extraction and purification,as well as chromatographic and mass spectrometric parameters were optimized. The samples were extracted by soxhlet with 100 m L hexane ∶ acetone（ V ∶V,50∶50）,and purified by molecular imprinted column（ MIPs/SPE）. The internal standard method was used for quantitative analysis. The results show that molecular imprinted column（ MIPs/SPE） has a significant effect on the adsorption of PAHs＇ monomer,and the adsorption of PAHs on central and high ring is obvious,and the matrix effect is weakened. The calibration curvesof 16 PAHs were linear in the range of 10—5000 ng·m L-1with correlation coefficients（ R^2） not less than 0.9978. The average spiked recoveries at the spiked levels of 50,250 and 500 ng·m L-1were in the range of 60%—105%,58%—121% and 63%—115%,respectively,with relative standard deviations（ RSDs,n = 6） in the range of 3.8%—9.4%.The results showed that the method is rapid,accurate,sensitive and reliable.