Citation: SHAN Guoqiang, YU Mengqi, YU Shengsong, ZHU Lingyan. Analysis of perfluorooctanoic acid by high performance liquid chromatography with 3,4-dichloroaniline derivatization[J]. Chinese Journal of Chromatography, ;2014, 32(9): 942-947. doi: 10.3724/SP.J.1123.2014.05028 shu

Analysis of perfluorooctanoic acid by high performance liquid chromatography with 3,4-dichloroaniline derivatization

1.
1. Key Laboratory of Pollution Processes and Environmental Criteria, Ministry of Education, Tianjin Key Laboratory of Environmental Remediation and Pollution Control, College of Environmental Science and Engineering, Nankai University, Tianjin 300071, China;

Corresponding author: ZHU Lingyan,
Received Date: 22 May 2014
Available Online: 15 July 2014
Fund Project: 国家自然科学基金项目(21077058) (21077058)天津市科技计划项目(12JCYBJC16000) (12JCYBJC16000)环境化学与生态毒理学国家重点实验室开放基金项目(KF2009-01). (KF2009-01)

A simple derivatization method followed by high performance liquid chromatography (HPLC) for the analysis of perfluorooctanoic acid (PFOA) was developed. PFOA was firstly derivatized with 3,4-dichloroaniline (DCA) using carbodiimide method. The typical amidate product was characterized by mass spectrometry (MS). It can be detected by a UV detector at maximum absorption wavelength of 255 nm. It was isolated well by methanol/H₂O (8/2, v/v) as mobile phase. The DCA derivatization of PFOA in organic or aqueous solutions was optimized. The following purification procedures with thin layer chromatography (TLC) and HPLC separations were established. Using external standard method with the authentic PFOA-DCA derivative as standard, the limit of instrumental quantification was found to be 0.5 mg/L. Good linear correlation coefficients were observed in 0.5-50.0 mg/L. The accuracy of the method was evaluated by the recovery measurements on spiked samples. The recoveries for the spiked samples (1.0 mg/L) in organic phase and aqueous phase were 91.8%-108.7% and 42.1%-53.7%, respectively. Comparing to the reported pre-column derivatization methods followed by HPLC for the determination of PFOA, this method has the advantages of mild reaction conditions, very stable derivative, easy operation, low cost, etc. The method was successfully applied for the quantification of PFOA in photodegradation experiments, and the results were consistent with those determined by LC/MS. Considering the combination of the preconcentration step, it has a potential for the application of the analysis of samples containing relatively low concentrations, such as μg/L levels of PFOA obtained from environmental or scientific experiments.
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