mass spectrometry and chromatography explained...mass spectrometry and chromatography explained...
TRANSCRIPT
![Page 1: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/1.jpg)
• Dr. Mark Strynar – US EPA • National Exposure Research Laboratory (NERL)
Mass Spectrometry and Chromatography Explained
February 21st, 2018Meeting of the House Select Committee on North Carolina River Quality
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Questions to Answer?• What is mass spectrometry?• What are the types of mass spectrometry
• (MS, MS/MS, QTOF, Orbitrap)• What is resolution in mass spectrometry?
(low resolution, high resolution, ultra-high resolution)• What is mass accuracy?• What is liquid and gas chromatography?• What can be done with each mass spectrometer?; i.e. targeted versus
non-targeted work• Questions I did not answer
![Page 3: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/3.jpg)
Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
What is Mass Spectrometry
O
O
OH
OHCH3O
CH3
H
H
H
Molecular Formula = C21H26O5Formula Weight = 358.42814Composition = C(70.37%) H(7.31%) O(22.32%)Monoisotopic Mass = 358.178024 DaNominal Mass = 358 DaAverage Mass = 358.4281 Da
Prednisone
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
• Chevy• Low resolution• Nominal mass• Inexpensive/common
• Cadillac• High resolution• Exact mass• More expensive/becoming
more common
![Page 5: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/5.jpg)
Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
• Tesla• Ultra-high resolution• Exact Mass/ Fine isotope structure• Significantly more expensive;
uncommon
The Thermo Scientific™ Orbitrap Fusion™ Tribrid™ mass spectrometer
![Page 6: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/6.jpg)
Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Resolution in mass spectrometry is the ability to differentiate a detected ion from any other
From Balough, LCGC 2004
What is resolution?
• Triple Quad or MS/MS 500-5,000 resolution• TOF or QTOF ~25,000 resolution• Orbitrap >250,000 resolution
Scales example.
Lab scale Bathroom Scale
![Page 7: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/7.jpg)
Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
LCGC North America Vol 22 Number 2 February 2004 MS The Practical Art Michael Balough “Debating Resolution and Mass Accuracy”
Mass Accuracy (Tune)
1633.9498 - 1633.9395 = 0.0103
0.0103 / 1633.9498 10^6 = 6.3 ppm
What is Mass Accuracy?
![Page 8: Mass Spectrometry and Chromatography Explained...Mass Spectrometry and Chromatography Explained February 21 st, 2018 Meeting of the House Select Committee on North Carolina River Quality](https://reader034.vdocument.in/reader034/viewer/2022042508/5f70d3b382f78836da060727/html5/thumbnails/8.jpg)
Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Single Quad MS
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
• MRM or transition• Parent to daughter
Ex. PFOA 413-369413-169
MS/MS or Triple Quad
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
FF
F
F
F
F
F
F
F
F
F
F
F
F
F
O
O-
C-FF
F
F
F
F
F
F
F
F
F
F
F
F
F
C-FF
F
F
F
F
F
Ex. PFOA
Q3 169
Q1 413
Q3 369
Q2
TARGETED ANALYSIS
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Ex. PFOA exact mass 412.9664 Da
FF
F
F
F
F
F
F
F
F
F
F
F
F
F
O
O-
TOFMSor
QTOFMS
C-FF
F
F
F
F
F
F
F
F
F
F
F
F
F
368.9766 Da
Targeted Analysis or Non-targeted AnalysisPost-analysis data mining
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Orbitrap
TARGETED ANALYSISNON TARGETED ANALYSISSTRUCTURE ELUCIDATIONPOST ANALYSIS DATA MINING
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
What is Liquid Chromatography; Gas Chromatography
Pump A (water)
Pump B (methanol)
Sample Mixture
Detector
High Pressure Liquid Chromatography (HPLC) column
Time
Response
****RT and response****
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Liquid Chromatography Gas Chromatography
Non-volatile chemicalsPolar chemicalsWater soluble chemicalsExample: PFOA, GenX, Nafion BP
Volatile chemicalsNon-Polar chemicalsWater soluble chemicalsExample: Benzene, formaldehyde, HFPO
VS
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Office of Research and DevelopmentNational Exposure Research Lab/ Human Exposure and Atmospheric Science Division
Work done in collaboration with NC DEQ summer/fall 2017 (GenX)
Targeted analysis of PFAS in water samples (MS/MS or Triple Quad analysis) resolution 500-5000 GenX, legacy PFAS (PFOS/PFOA)
Non-targeted analysis of PFAS in water samples (TOFMS analysis) resolution 25,000Nafion BP1, Nafion BP2, PFMOAA, PFO2HxA, PFO3OA, other previously undescribed analytes