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Dioxin/Furan Screening Method

Dioxin/Furan Screening Method. John D. Ragsdale, GC/MS Product Specialist. GC/MS/MS Dioxin Screening. In The Beginning… Current Methodology The Plan Sample Preparation The GC/MS/MS Configuration The data. In The Beginning….

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Dioxin/Furan Screening Method

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  1. Dioxin/Furan Screening Method John D. Ragsdale, GC/MS Product Specialist

  2. GC/MS/MS Dioxin Screening • In The Beginning… • Current Methodology • The Plan • Sample Preparation • The GC/MS/MS Configuration • The data

  3. In The Beginning… Interest in the analysis of dioxins and furans have increased due to the contamination of feed for livestock and poultry in Europe. The local sales force has responded by requesting application notes and other literature for this analysis on PolarisQ. Similar requests have come from our Pan-Pacific and Asian sales force. This group also includes a current Finnigan customer directly involved in the analysis of dioxin and furan contaminated samples.

  4. Low Resolution MS 8270 ( full scan ) 8280 ( SIM ) Part per million and part per billion detection limits High Resolution MS 8290 ( SIM ) 1613 ( SIM ) Part per trillion detection limits Dioxin/Furan Analysis EPA Methods

  5. Sample Preparation Minimal cleanup required Chromatographic Resolution BPX-5; 25M; 0.15mm ID column Robust Chromatography Split injections (2 ul injection) Specificity MS/MS Deliverables Write SOPs The Plan

  6. Sample Preparation • 25 grams of material mixed with 50 grams of sodium sulfate. • Soxhlet extraction for 24 hours with 50:50 hexane : methylene chloride. • Partition against 4 X 40ml concentrated sulfuric acid. • Concentrate to 100 ul of 5X dilution of CS3 (2pg/ul of tetra-isomers)

  7. Additional Sample Preparation Any additional cleanup will lower ultimate detection limits but is not required for this MS/MS screening technique • Gel Permeation Chromatography • Removes high molecular weight interferences • Acid, neutral, and basic silica gel and carbon • Removes nonpolar and polar interferences • Alumina, Florosil • Removes chlorodiphenyl ethers

  8. Dioxin Screening GC/MS/MS System • Trace GC with split/splitless inlet • PPKD DPFC 700kPa with Manual Split Flow • 250 Liter Turbo pump • PolarisQ EI only / Vacuum Interlock • AS2000 Liquid Autosampler • SGE BPX-5, 25 meter, 0.15 mm ID, 0.25 micron film column • Restek Silco-Steel split liners w/glass wool plug

  9. Split Injections allow for “dirtier” sample introduction. Extracts can be screened without the time and cost of extensive cleanup. MS/MS affords the selectivity to remove matrix interference from “dirty” extracts. Configuration Rationale

  10. Chromatographic Conditions • Injector: • 250C • Column Flow: • 0.9 ml/min • Split flow: • 10 ml/min • Ramp: • 150C (1min) to 200C @ 20C/min (1.5min) • to 300C @ 3C/min (1.7min) : 40min total

  11. Tetra-Dioxins Tetra-Furans Chromatographic Resolution 2,3,7,8 TCDD 2,3,7,8 TCDF 2,3,7,8 TCDD-IS 2,3,7,8 TCDF-IS

  12. Full Scan, SIM, or MS/MS

  13. Full Scan – 10pg/ul in 25g Cow’s milk

  14. Dioxins: EPA Method 1613 • Linearity to 500 fg/uL to 200 pg/uL for 2,3,7,8-TCDD

  15. Dioxins: Typical 500 fg/ul injection

  16. Dioxins:Typical Precision for 1613

  17. Dioxins:Typical Precision for 1613 ISTD

  18. Dioxins: Isotope Ratio Stability

  19. Dioxins: Full Scan – 10pg/ul std vs. cow’s milk 2,3,7,8 TCDD 2,3,7,8-TCDD ?? 2,3,7,8 TCDD-IS 2,3,7,8 TCDD-IS 1,2,3,4 TCDD-RS 1,2,3,4 TCDD-RS Cow’s milk Nonane

  20. Dioxins: MS/MS – 10pg in nonane 2,3,7,8 TCDD 2,3,7,8 TCDD-IS 1,2,3,4 TCDD-RS

  21. Dioxins: MS/MS – 10pg/ul in cow’s milk 2,3,7,8 TCDD 2,3,7,8 TCDD-IS 1,2,3,4 TCDD-RS

  22. Furans: EPA Method 1613 Linearity from 500 fg/uL to 200 pg/uL for 2,3,7,8-TCDF

  23. Furans: Typical 500 fg/ul Injection

  24. Furans:Typical Precision for 1613

  25. Furans:Typical Precision for 1613 ISTD

  26. Furans: Isotope Ratio Stability

  27. Furans: Full Scan – 10pg/ul std vs. cow’s milk 2,3,7,8 TCDF 2,3,7,8 TCDF ??? 2,3,7,8 TCDF-IS 2,3,7,8 TCDF-IS Cow’s Milk Nonane

  28. Furans: MS/MS – 10pg/ul in nonane 2,3,7,8 TCDF 2,3,7,8 TCDF-IS

  29. Furans: MS/MS – 10pg/ul in cow’s milk 2,3,7,8 TCDF 2,3,7,8 TCDF-IS

  30. Cow’s milk Soil Coal fly ash Spiked Matrix @ 2pg/ul or 4 pg/g (ppt)

  31. Dioxin: 2 pg/ul in 25g Cow’s Milk 2,3,7,8 TCDF 2,3,7,8 TCDD 2,3,7,8 TCDF-IS 1,2,3,4 TCDD-RS 2,3,7,8 TCDD-IS TCDF TCDD

  32. Dioxin: 2 pg/ul in 25g Soil 2,3,7,8 TCDF 2,3,7,8 TCDD 2,3,7,8 TCDF-IS 1,2,3,4 TCDD-RS 2,3,7,8 TCDD-IS TCDF TCDD

  33. 2 pg/ul in 25g Coal Fly Ash 2,3,7,8 TCDF 2,3,7,8 TCDD 2,3,7,8 TCDF-IS 1,2,3,4 TCDD-RS 2,3,7,8 TCDD-IS TCDF TCDD

  34. Summary of analyte recovery 2,3,7,8-TCDD (2 pg/ul spike) 2,3,7,8-TCDF (2 pg/ul spike)

  35. Summary of isotope ratios 2,3,7,8-TCDD 259/257 2,3,7,8-TCDF 243/241

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