Cost-Effective Detection of Perfluoroalkyl Carboxylic Acids with Gas Chromatography: Optimization of Derivatization Approaches and Method Validation

衍生化 色谱法 化学 萃取(化学) 固相萃取 气相色谱法 气相色谱-质谱法 样品制备 检出限 高效液相色谱法 质谱法
作者
Zhen Li,Hongwei Sun
出处
期刊:International Journal of Environmental Research and Public Health [Multidisciplinary Digital Publishing Institute]
卷期号:17 (1): 100-100 被引量:6
标识
DOI:10.3390/ijerph17010100
摘要

The reliable quantification of perfluoroalkyl carboxylic acids (PFCAs) in environmental samples like surface water by using gas chromatography (GC) remains challenging because the polar PFCAs call for derivatization before injection and problems involving the integration of sample pretreatment and derivatization procedures. Here we proposed a cost-effective method for the GC based determination of C4–C12 PFCAs in surface water samples by integrating solid phase extraction and PFCAs anilide derivatization. First, we assessed the performance of different PFCAs derivatization methods, namely esterification and amidation. Esterification was unable to derivatize C4–C6 PFCAs. On the contrary, amidation procedures by using 2,4-difluoroaniline (DFA) and N,N′-dicyclohexylcarbodiimide (DCC) could successfully transform all the PFCA analogs to produce anilide derivatives, which could be easily detected by GC. Then the reaction conditions in the amidation approach were further optimized by using orthogonal design experiments. After optimizing the instrumental parameters of GC, the limits of detection (LOD) of this derivatization method were determined to be 1.14–6.32 μg L−1. Finally, in order to establish an intact method for the quantification of PFCAs in surface water samples, solid phase extraction (SPE) was used for extraction and cleanup, which was further integrated with the subsequent amidation process. The SPE-amidation-GC method was validated for application, with good accuracy and precision reflected by the PFCAs recoveries and derivatization of triplicates. The method reported here could provide a promising and cost-effective alternative for the simultaneous determination of C4–C12 PFCAs in environmental water samples.

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