Supplemental quality assurance criteria for high-resolution gas chromatography/high-resolution mass spectrometric determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in biological tissue

Journal Article · Sun Jun 01 00:00:00 EDT 1986 · Anal. Chem.; (United States)

DOI:https://doi.org/10.1021/ac00298a082· OSTI ID:5569906

Kuehl, D W; Butterworth, B C; Johnson, K L

During the past 2 years our laboratories have been responsible for the analysis of nearly 2000 fish tissue samples for part-per-trillion levels of 2,3,7,8-tetrachlorodibenzo-p-dioxins (2,3,7,8-TCDD) through both our in-house toxicology studies and the US EPA National Dioxin Study. Three areas of concern in 2,3,7,8-TCDD analysis are (1) mass resolution, (2) chromatographic isomer specificity, and (3) minimum level of detection. Currently practiced analytical procedures and quality assurance plans describe only techniques to establish or verify instrumental parameters prior to or after TCDD analyses. These methods primarily utilize (/sup 13/C/sub 12/)2,3,7,8-TCDD and (/sup 37/Cl/sub 4/)2,3,7,8-TCDD to conduct an isotope dilution mass spectrometry experiment and the 22 TCDD isomers to establish gas chromatographic isomer specificity. Mass spectrometer resolution is most often established by using a reference mixture such as perfluorokerosene. The authors have synthesized (/sup 13/C/sub 6/)1,2,3,4-TCDD (Cambridge Isotope) and have purchased 1,2,3,4-TCDD (Supelco). The use of these additional standards, along with the others previously mentioned, allows for the development of quality assurance criteria for the measurement of mass resolution, chromatographic resolution, and minimum level of detection during each TCDD GC/MS analyses. The method developed for the cleanup of biological tissue samples is capable of isolating many polychlorinated dibenzo-p-dioxins (PCDDs) in addition to 2,3,7,8-TCDD.

• Research Organization: Environmental Protection Agency, Duluth, MN
• OSTI ID: 5569906
• Journal Information: Anal. Chem.; (United States), Vol. 58:7
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
BIOLOGICAL MATERIALS
QUANTITATIVE CHEMICAL ANALYSIS
DIOXIN
GAS CHROMATOGRAPHY
MASS SPECTROSCOPY
EXPERIMENTAL DATA
QUALITY ASSURANCE
RESOLUTION
TRACE AMOUNTS
CHEMICAL ANALYSIS
CHROMATOGRAPHY
DATA
HETEROCYCLIC COMPOUNDS
INFORMATION
MATERIALS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
SEPARATION PROCESSES
SPECTROSCOPY
400102* - Chemical & Spectral Procedures
400104 - Spectral Procedures- (-1987)