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Travelling Wave Ion Mobility Studies of Polymer
Microstructure
Jim Scrivens
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Challenges in characterising polymer
formulations• Extremely complex mixtures• Variation of starting materials• Poorly controlled reactions• Molecular weight range• Sold on properties not structure• Chromatographic separation
difficult
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Requirement
• Rapid analysis• High information content• Molecular weight and structural
information• Ability to differentiate small
differences in complex formulations
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Ion mobility platforms
• Drift cell– Currently predominately academic based
• Differential mobility spectroscopy (DMS)– Includes FAIMS– Theory challenging
• Travelling wave– Commercially available– Theory challenging
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Ion mobility issues
• Sensitivity• Speed • Selectivity• Ease of use• Resolution• Availability
• Information content
• Reproducibility• Calibration• Cost• Data analysis
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References
• Ion mobility–mass spectrometry– Abu B. Kanu, Prabha Dwivedi, Maggie Tam, Laura Matz and Herbert H.
Hill Jr.– J. Mass Spectrom. 2008; 43: 1–22
• Differential Ion Mobility Spectrometry: Nonlinear Ion Transport And Fundamentals Of FAIMS– Alexandre A Shvartsburg– CRC Press, ISBN: 9781420051063, 2008
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Travelling Wave References
• An investigation of the mobility separation of some peptide and protein ions using a new hybrid quadrupole/travelling wave IMS/oa-ToF instrument– Steven D. Pringle , Kevin Giles , Jason L. Wildgoose , Jonathan P.
Williams , Susan E. Slade , Konstantinos Thalassinos , Robert H. Bateman , Michael T. Bowers and James H. Scrivens
– International Journal of Mass Spectrometry, 261, 1-12, 2007
• Applications of Travelling Wave Ion Mobility-Mass Spectrometry – Konstantinos Thalassinos and James H Scrivens– Practical Aspects of Trapped Ion Mass Spectrometry Volume 5, 2009
• Special issue of IJMS on Ion Mobility– Edited by Richard Yost, James Scrivens– IJMS, 2010
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Pringle, S. D. et al., International Journal of Mass Spectrometry, 261, 1-12, 2007Thalassinos K and Scrivens J H, “Applications of Travelling Wave Ion Mobility-Mass Spectrometry”, Practical Aspects of Trapped Ion Mass Spectrometry Volume 5
Schematic of Synapt G1
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Features of Synapt
• Ease of use
• Rapid analysis (typically 200 spectra in 18ms)
• High sensitivity (fmole)
• Can acquire MS, MS/MS with accurate mass data
• Estimated relative cross-sections can be obtained by use of calibration against known standards
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Aspirations
• Higher mobility resolution
• Better dynamic range
• Higher resolution mass spectrometry
• No compromise in: -– Sensitivity– Speed– Ease of use
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Schematic of Synapt G2
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TOF developments
QuanTof improvements— High field pusher — Dual stage reflectron — Hybrid ion detection system — compatible with UPLC separations— compatible with HDMS analysis
Performance— Resolution – over 40,000 FWHM— Mass Measurement – 1ppm RMS— Dynamic Range – up to 105
— Speed - 20 Spectra/sec
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Mobility Cell improvements
Second generation Triwave device— Increased ion mobility
resolution (over 40 Ω/ΔΩ) IMS cell 40% longer Higher gas pressure in IMS T-
Wave (2.5mb versus 0.5mb) Modified T-Wave pattern - use of
Higher T-Wave pulse amplitudes/fields
Helium cell balances N2
pressure in Maximizes transmission of ions on entry into the mobility cell
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Rabbit haemoglobin peptide Synapt G1
20 40 60 80 100 120 140 160 180 200Scan
99
84
115
81
76 m/z 977
m/z 857
m/z 1037
m/z 1134
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Rabbit haemoglobin peptide Synapt G2
20 40 60 80 100 120 140 160 180 200Scan
102
89
110
86
84 m/z 977
m/z 857
m/z 1037
m/z 1134
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Rabbit haemoglobin peptide ATD comparison
20 40 60 80 100 120 140 160 180 200Scan
99
84
81
76
102
89
86
84
Synapt G2
m/z 977
m/z 857
m/z 1037
m/z 1134
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Positive ion [M+Na]+ ESI mass spectrum of N-glycans released from chicken
ovalbumin
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Ion mobility separations of positive ions [M+Na]+ of N-glycans released from chicken ovalbumin with
compositions of Hex3GlcNAc2 Hex3GlcNAc3 (two isomers) and Hex3GlcNAc4
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Ion mobility separations of positive ions [M+Na]+ of N-glycans released from chicken ovalbumin with compositions of Hex3GlcNAc2 Hex3GlcNAc3 (two
isomers) and Hex3GlcNAc4
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Positive ion [M+Na]+ ion mobility MS/MS spectra of the first and second N-glycan isomers of m/z 1136
from chicken ovalbumin
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EESI of aerosol formulations
Sample
Sample headspace
Solvent
Desolvation Gas plus analyte
Sample molecules
Charged solvent droplets
Desolvation Gas plus analyte
Sample Container
Mass Spectrometer
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Carbomethoxypyridines
N
O
CH3
O
N
O
CH3
O
N
O
CH3
O
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Mobility separation of isomers
Methyl Picolinate 1/200 dilution 138 MS/MS transfer, 2000WV
Scan10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
%
0
100
10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
%
0
100
10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200
%
0
100
WAR112409_09_dt_01 Sm (SG, 2x3) TOF MSMS ES+ 137.6_138.5
1.70e4100
WAR112409_14_dt_01 Sm (SG, 2x3) TOF MSMS ES+ 137.9_138.2
2.21e499
WAR112409_11_dt_01 Sm (SG, 2x3) TOF MSMS ES+ 138_138.1
2.27e493
Para
Meta
Ortho
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ATD for isomers
OrthoPara
Meta
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Isobaric PEG systems
• Oligomers of di-hydroxyl end-capped PEG & PEG monooleate have same nominal mass-to-charge ratio – Different number of moles of ethylene oxide (EO)
• Resolution required to separate oligomers is ~6300
• Difference in m/z for two oligomers is 0.0880
– m/z 553.3411
– m/z 553.4292
12
O CH2CH2 OHH
6
CH3 (CH2)6 CH2 CH CH CH2 (CH2)5 CH2 C O CH2CH2 O H
O
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Synapt G1 mobility separation – m/z 553
20 40 60 80 100 120 140
Scan
100 200 300 400 500m/z
100 200 300 400 500m/z
12
O CH2CH2 OHH6
CH3 (CH2)6 CH2 CH CH CH2 (CH2)5 CH2 C O CH2CH2 O H
O
[M+Li]+
[M+Li]+
Hilton G. R., et al,. Anal. Chem., 2008, 80 (24), 9720-9725
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Synapt G1 mobility separation – m/z 861
50 60 70 80 90 100110120130140150Scan
100 200 300 400 500 600 700 800 900m/z 100 200 300 400 500 600 700 800 900m/z
19O CH2CH2 OHH
13CH3 (CH2)6 CH2 CH CH CH2 (CH2)5 CH2 C O CH2CH2 O H
O
[M+Li]+
[M+Li]+
Hilton G. R., et al,. Anal. Chem., 2008, 80 (24), 9720-9725
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Synapt G2: Ion mobility separation – m/z 1126
Scan120 130 140 150 160 170 180 190 200
m/z200 400 600 800 1000
18O CH2CH2 OHH
25
m/z200 400 600 800 1000
12CH3 (CH2)6 CH2 CH CHCH2 (CH2)5 CH2 C O CH2CH2 O H
O
19
[M+Li]+[M+Li]+
Precursor ion resolution8434
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Driftscope separation G2
PEG 1000
PEG mono oleate
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Synthesis of Tween 20
[C2H4O]nO+
- H2O +
IsosorbideSorbitan
- H2O
Sorbitol
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Structures of Tween formulations
Formulation Structure Indicated purity
Tween 20 Polyoxyethylene (20) sorbitan monolaurate
50%
Tween 40 Polyoxyethylene (20) sorbitan monopalmatate
90%
Tween 60 Polyoxyethylene (20) sorbitan monostearate
50%
Tween 80 Polyoxyethylene (20) sorbitan monooleate
70%
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Structures of major products
Sorbitan polyethoxylate [SPE]Isosorbide polyethoxylate [SPE]
Polysorbate monoester [PME]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OCR
H2CH2COHO
W
X
Y
Z
O
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OH
H2CH2COHO
W
X
Y
Z
O
O
OCH2CH2
H2CH2CO
OH
HO
M
P
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Tween 20 overall averaged spectrum
m/z200 400 600 800 1000 1200 1400
%
0
100617.4
595.4573.3
410.2
223.2
141.1
388.2
686.4
708.5
752.5
774.5
775.5819.5821.5
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Major species Tween 20
Series 1
686.4 + n*22Li2 [2+]R = C11H23 [laurate]
686*2 = 13721372 – 14 [Li2] = 13581358 – 164 [sorbitan] = 11941194 – 182 [RCOOH – H2O] = 10121012/44 [CH2CH2O] = 23
W + X + Y + Z = 23
Polysorbate monoester [PME]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OCR
H2CH2COHO
W
X
Y
Z
O
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Major species Tween 20
Series 2
573.3 + n*22Li2 [2+]
573*2 = 11461146 – 14 [Li2] = 11321132 – 164 [sorbitan] = 968968/44 [CH2CH2O] = 22
W + X + Y + Z = 22
Sorbitan polyethoxylate [SPE]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OH
H2CH2COHO
W
X
Y
Z
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Major species Tween 20
Series 3
322 + n*22Li2 [2+]
322*2 = 644644 – 14 [Li2] = 630630 – 146 [isosorbide] = 484484/44 [CH2CH2O] = 11
P + M = 11
Isosorbide polyethoxylate [SPE]
O
O
OCH2CH2
H2CH2CO
OH
HO
M
P
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Tween 20 mobility separationWAR112409_28A.raw : 1
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Tween 20 mobility separation
WAR112409_28A.raw : 1
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Tween 20 mobility separationWAR112409_28A.raw : 1
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Tween 20 MALDI spectrum
Isosorbide polyethoxylate [SPE]Sorbitan polyethoxylate [SPE]
Polysorbate monoester [PME]
Folahan O Ayorinde et al Rapid Comm. Mass Spectrom, 14, 2116, (2000)
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m/z400 600 800 1000 1200 1400
%
0
100692.5
670.4
595.4
537.4
485.3
410.2
736.5
758.5
759.0
781.0
803.0
875.6
921.6
Tween 40 overall averaged spectrum
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Major series Tween 40
Series 1
670.4 + n*22Li2 [2+]R = C15H31 [palmitate]
670*2 = 13401340 – 14 [Li2] = 13261326 – 164 [sorbitan] = 11621162 – 238 [RCOOH – H2O] = 924924/44 [CH2CH2O] = 21
W + X + Y + Z = 21
Polysorbate monoester [PME]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OCR
H2CH2COHO
W
X
Y
Z
O
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Major series Tween 40
Series 2
573.3 + n*22Li2 [2+]
573*2 = 11461146 – 14 [Li2] = 11321132 – 164 [sorbitan] = 968968/44 [CH2CH2O] = 22
W + X + Y + Z = 22
Sorbitan polyethoxylate [SPE]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OH
H2CH2COHO
W
X
Y
Z
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Major series Tween 40
Series 3
322 + n*22Li2 [2+]
322*2 = 644644 – 14 [Li2] = 630630 – 146 [isosorbide] = 484484/44 [CH2CH2O] = 11
P + M = 11
Isosorbide polyethoxylate [SPE]
O
O
OCH2CH2
H2CH2CO
OH
HO
M
P
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WAR112409_29.raw : 1
Tween 40 mobility separation
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WAR112409_29.raw : 1
Tween 40 mobility separation
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Tween 40 extracted regionsWAR112409_29.raw : 1
A
B
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Tween 40 conformational families
m/z500 550 600 650 700 750 800
%
0
100
%
0
100692.5
670.4
669.9
714.5
758.5780.5
802.5 824.5
573.3551.3
529.3507.3
595.4
617.9
639.9
647.4
A
B
Polysorbate monoester [PME]
Sorbitan polyethoxylate [SPE]
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OCR
H2CH2COHO
W
X
Y
Z
O
O
OCH2CH2 OH
OCH2CH2
OCH2CH2 OH
OH
H2CH2COHO
W
X
Y
Z
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Tween 40 extracted regions
WAR112409_29.raw : 1
a
b
c
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m/z600 700 800 900 1000 1100 1200 1300
%
0
100
%
0
100
%
0
1001025.8981.7
893.7849.7
1069.8
1157.81201.9
831.6743.5
699.5
615.5
875.6
963.6 1007.71201.8
1051.6963.6919.5
901.5900.5
1095.61183.7
1271.71315.8
c
b
a
Tween 40 conformational families
Polysorbate monoester [PME]
Polyisosorbide monoester [PME]
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Tween 40 MALDI spectrum
Isosorbide polyethoxylate [SPE]
Sorbitan polyethoxylate [SPE]
Polysorbate monoester [PME]
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m/z400 600 800 1000 1200 1400
%
0
100595.4
451.1
443.3
428.6
692.5728.5
736.5
758.5
773.0
802.5817.0
Tween 60 overall averaged spectrum
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WAR112409_30.raw : 1
Tween 60 mobility separation
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Tween 60 MALDI spectrum
Isosorbide polyethoxylate [SPE]
Sorbitan polyethoxylate [SPE]
Polysorbate monoester [PME]
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Tween 80 overall averaged spectrum
m/z400 500 600 700 800 900 1000 1100 1200 1300
%
0
100x2x2
525.1
575.4 771.5604.7619.7
815.5
860.1
925.6
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Tween 80 mobility separationWAR112409_31.raw : 1
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Tween 80 MALDI spectrum
Isosorbide polyethoxylate [SPE]
Sorbitan polyethoxylate [SPE]
Polysorbate monoester [PME]
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Conclusions
• ESI mobility-separated spectra offer an excellent screening approach for complex polymer formulations
• A number of, previously unseen, conformational series may be observed and extracted
• Mobility-separated MS/MS data can provide more detailed structural information
• The ESI spectra show greater agreement with published compositions than those obtained using MALDI
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BMSP research group