不同研究报道的空气中离子型全氟化合物(PFCs)的分析方法各不相同,本文的目的在于对比和优化不同分析条件。通过对比不同流动相(甲醇和乙腈)、不同色谱柱(C8和C18)、不同梯度洗脱条件下目标化合物的分离效果,确定了以甲醇为流动相、C18色谱柱为分离柱和最佳梯度淋洗液分离的仪器分析条件。比较了甲醇和正已烷/丙酮混合溶剂萃取气相(PUF)和颗粒相(GFF)样品的效果,确定以甲醇为萃取溶剂。建立了空气中PFCs的LC-MS/MS优化分析方法,方法线性范围在0.1~50 ng·m L^(-1)之间,PUF与GFF样品方法检出限分别为0.02~0.35 pg·m^(-3)和0.02~0.26 pg·m^(-3)。同时将方法用于大气实际样品分析。
Various methods have been used to analyze perfluorinated compounds(PFCs) in atmospheric samples.The analytical conditions such as mobile phases of methanol and acetonitrile, chromatographic columns of C8 and C18, and different gradient elution methods were tested in the present work. The results suggested that best separation efficiency could be obtained when methanol was used as mobile phase on C18 chromatographic column with optimized gradient elution method. Methanol was selected as the extraction solvent, since it was more efficient to extract PFCs from both gas phase(polyurethane foam) and particle phase(glass fiber filter) samples than n-hexane/ac-etone mixture. An optimized method for determination of PFCs in ambient air on LC-MS/MS was established in this study, with a linearity range of 0.1 to 50 ng·m L-1. The method detection limit ranged from 0.02 to 0.35 pg·m-3for PUF samples and from 0.02 to 0.26 pg·m-3for GFF samples, respectively. This method was also applied to analyze PFCs in field atmospheric samples.