US EPA

6506099 

Journal Article 

Derivatization of Perfluorocarboxylic Acids with N,N-Dimethylformamide Dimethylacetal Prior to GC-MS Analysis 

Strozynska, M; Schuhen, K 

2020 

Yes 

Chromatographia
ISSN: 0009-5893
EISSN: 1612-1112 

83 

3 

477-482 

10.1007/s10337-019-03850-6 

WOS:000516554500012 

A simple derivatization reaction with N,N-dimethylformamide dimethyl acetal (DMF-DMA) was developed for the analysis of perfluorocarboxylic acids (PFCA, C4-C12) in solid samples by gas chromatography-mass spectrometry (GC-MS). After extraction with methyl tert-butyl ether (MTBE), the samples are mixed with derivatizing agent and injected into GC. The derivatization reaction takes place in injection block forming corresponding N,N,N ',N '-tetramethyl diamines. The method provides excellent separation of nine PFCA (C4-C12) in 15 min and is characterized by good precision (max. RSD = 6.21% for 10 ng/mL, n = 6), linearity and detection limits in the range of 0.15-0.38 ng/mL. The main aim of the study was to develop a quick and easy GC-MS screening for PFCA. The method was successfully applied for sewage sludge, textiles and dental flosses. To confirm the laboratory evaluation, two samples were measured by an external laboratory using LC-MS/MS and showed comparable results. The proposed method is very promising, taking into account its simplicity, mild conditions and application of cost-effective GC-MS system. Additionally, a comparison with two other derivatization methods for PFCA: reaction with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and benzyl bromide is presented. 

Dimethylformamide dimethyl acetal (DMF-DMA); Perfluorocarboxylic acids; PFOA; Gas chromatography-mass spectrometry; Derivatization