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Analysis of Perfluorinated Compounds (PFCs) by Liquid Chromatography/Mass Spectrometry Jia Wang April 11, 2013.

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Presentation on theme: "Analysis of Perfluorinated Compounds (PFCs) by Liquid Chromatography/Mass Spectrometry Jia Wang April 11, 2013."— Presentation transcript:

1 Analysis of Perfluorinated Compounds (PFCs) by Liquid Chromatography/Mass Spectrometry Jia Wang April 11, 2013

2 2 Perfluorinated Compounds Stain, oil and water resistant Chemical and thermo stability Applied to fabrics, papers, carpets, and fire-fighting foam Persistent, bioaccumulative and toxic PFOA and PFOS now on CCL3 list (Contaminant Candidate List 3)

3 3 EPA Method 537

4 4 Lancaster Laboratories and Thermo Fisher Scientific Participated in the Second Laboratory Demonstration of EPA Method 537

5 5 Compounds Analyzed * Technical Grade: both linear and branched isomers

6 6 Mobile phase: 20 mM ammonium acetate and methanol Injection solvent: 96:4% (vol/vol) methanol:water Injection volume: 10 L Flow rate: 0.3 mL/min Electrospray ionization (ESI): Negative LC gradient Time (min)% 20 mM ammonium acetate% Methanol EPA Method 537 LC and ESI-MS Conditions

7 7 Sample Preparation Preservation reagent: Trizma® Preset Crystals, pH 7.0, 1.25 g/250 mL 250 mL water fortified with surrogates is extracted by SPE and eluted by methanol SPE cartridges: styrenedivinylbenzene (SDVB) sorbent, 0.5g/6mL The extract was concentrated to dryness and then adjusted to a 1 mL volume with 96:4% (vol/vol) methanol: water

8 8 PFCs Analysis Challenge Method interferences may be caused by contaminants in solvents, reagents, sample bottles and caps, and other sample processing hardware that lead to discrete artifacts and/or elevated baselines in the chromatograms. The method analytes in this method can also be found in many common laboratory supplies and equipment, such as PTFE (polytetrafluoroethylene) products, LC solvent lines, methanol, aluminum foil, SPE sample transfer lines, etc. All items such as these must be routinely demonstrated to be free from interferences (less than 1/3 the MRL for each method analyte) under the conditions of the analysis by analyzing laboratory reagent blanks. Subtracting blank values from sample results is not permitted.

9 9 Thermo PFOA Analysis Kit

10 10 LC System Modification PTFE solvent frits and tubing were replaced by PEEK solvent frits and tubing Degasser was replaced by PFOA free degasser A trapping column (Thermo BDS-Hypersil, C8, 3 x 150 mm, 5 m) was placed between the pump outlet module and autosampler to trap and separate PFCs contaminant from analytes

11 11 Instrument: Thermo Fisher Scientific Dionex XRS Pump, Accela Open Autosampler, and TSQ Quantum Vantage Analytical Column: Thermo Scientific Accucore C18 column (3 x 150 mm, 2.6 m) Mobile phase: 20 mM ammonium acetate and methanol Electrospray ionization (ESI): Negative Time (min)% 20 mM ammonium acetate% Methanol LC and ESI MS Conditions

12 12 PFC Contaminants are Separated from Analytes ppb PFBS PFHxA PFHxA-SUR PFHpA PFHxS* PFOA * Technical grade PFOA Contaminant

13 13 PFC Contaminants are Separated from Analytes ppb PFOA-IS PFNA PFOS* PFOS-IS PFDA PFDA-SUR NMeFOSAA-IS * Technical grade

14 14 PFC Contaminants are Separated from Analytes ppb NMeFOSAA PFUnA NEtFOSAA-SUR NEtFOSAA PFDoA PFTrDA PFTA

15 15 PFC acquisition and analysis was performed using software with built-in workflows for streamlining method development and routine analysis. TraceFinder Software

16 16 Compound Database

17 17 Method Development

18 18 Method Development

19 19 Data Review – PFOA

20 20 Data Review – PFOS

21 21 Data Review – PFOS

22 22 Report View

23 23 Unregulated Contaminant Monitoring Rules 3 (UCMR3)

24 24 UCMR 3 Contaminants and Corresponding Analytical Methods - PFCs

25 25 Thermo Has Helped Customer to Receive UCMR3 Certification for EPA Method 537 EPA coordinates a Laboratory Approval Program for the contaminants. UCMR 3 requires laboratories have EPA approval to analyze PWS samples. Thermo Fisher Scientific has developed TraceFinder method for EPA method 537 UCMR3 analysis. Our customer has used this TraceFinder method for EPA method 537 UCMR3 application and PT samples analysis, and received EPA certification

26 26 Thermo Fisher Scientific offers PFOA analysis kit to reduce and separate PFCs contaminants from analytes Thermo Fisher Scientific and Lancaster Labs had previously participated in the second laboratory demonstration of EPA Method 537 Thermo Fisher Scientific has developed TraceFinder method for EPA method 537 UCMR3 analysis. Customer has used this TraceFinder method for EPA method 537 UCMR3 analysis and received EPA certification Summary

27 27 Thank You for Your Attention Questions?


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