Protocol for the Analysis of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry

摘要

An analytical protocol for the determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and total TCDDs in soil, sediment and aqueous samples using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) was developed using the best features of several candidate methods and input from experts in the field. Preliminary tests led to refinements of the chromatographic cleanup procedures and corresponding changes in the protocol. A final single-laboratory evaluation of the refined protocol, consisting of triplicate analyses of five solid and five aqueous samples showed that the method is useful for the determination of 2,3,7,8-TCDD and total TCDDs at concentrations from 10 to 200 pg/g (ppt) in soils and 100 to 2,000 pg/L (ppq) in aqueous samples. Based on the data generated and on the evaluation of several options, parts of the protocol were modified at the EMSL-LV to lower the quantitation limit for TCDD to 2 ppt in soil/sediments and to 20 ppq in aqueous samples.