presentation slides: two years on: the impact of orbitrap ...€¦ · 1 the world leader in serving...
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1 The world leader in serving science
NACRW 2017 Paul Silcock, Sr. Marketing Manager Orbitrap GC-MS PP10570
Two Years On: The Impact of Orbitrap™ GC-MS in Food Analysis
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Orbitrap Mass Analyzer
zmk/
=ω
• Ions injected into the Orbitrap are trapped in an electrostatic field
• Each ion oscillates axially with a frequency that is proportional to its mass
• An image current of these oscillations is measured using a split outer electrode
• This image is then converted to a mass spectrum using Fourier transform
• The longer a signal (transient) is measured, the higher the resolution
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ASMS 2015
A fully-integrated GC Orbitrap system 0pens a new chapter in GC-MS Paul Silcock1; Cristian Cojocariu1; Dominic Roberts1; Scott T. Quarmby2; G.Brody Guckenberger2; Jason S. Cole2; John G. Voss2; Amelia Peterson3; Jan-Peter Hauschild3; Oliver Lange3; Nicholas Kwiecien4; Michael S. Westphall4; Joshua J. Coon4; Alexander Makarov3
1Thermo Fisher Scientific, Runcorn, United Kingdom; 2Thermo Fisher Scientific, Austin, TX; 3Thermo Fisher Scientific, Bremen, Germany; 4University of Wisconsin, Madison, WI
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Redefining Routine GC-MS
RP 60,000 (FWHM @ m/z 200)
EI (VeV) / CI; Full-scan; Timed-SIM
NACRW 2016: Exactive™ GC Orbitrap™ GC-MS System
Orbitrap GC-MS family
ASMS 2015: Q Exactive™ GC Orbitrap™ GC-MS/MS System
Unprecedented Depth in Analysis
RP 120,000 (FWHM @ m/z 200)
EI (VeV) / CI; Full-scan, Timed-SIM
MS/MS capability
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EI 70eV VeV
Orbitrap GC system highlights
Sensitivity Mass Accuracy Resolving Power Dynamic Range
Up to 120,000 at m/z 200
< 1ppm ppt >6 orders
Harder Softer
CI
Ionization Range
• Standard library searchable spectra
• Molecular ion confirmation (incl. adducts)
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“Orbitrap spectra are not library searchable”
Mythbusting
“Orbitrap is too slow for GC”
Resolution
at
m/z 200
Transient
length,
(ms)
Scan
Rate,
Hz
15 000 32 22
30 000 64 14
60 000 128 7.4
120 000 256 3.5 Dieldrin 100pppb in baby food 60,000 RP (m/z 200)
2.4 s peak 60k RP
1 2
3
4
5
6
7
8 9
10
11
12
13
14
15 16 17
17 scans
Lanosterol TMS
Q Exactive GC
NIST
Compound NIST SI GC QToF
NIST SI Orbitrap
124-trichlorobenzene 890 834
Nitrobenzene 776 871
HCB 930 811
Acenaphtene 924 901
Aniline 730 715
2-Chlorophenol 745 842
1,3- Dichlorobenzene 930 900
Hexachlorethane 930 924
Hexachlorbutadiene 936 940
Average 866 860
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The impact of Orbitrap GC-MS in food analysis
Orbitrap HRAM Mass
Spectrometry Pesticide Residues
Authenticity Food Contact Materials
Persistent Organic Pollutants
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Instrument Detection Limits (Orbitrap vs. Triple Quad)
IDL ppb IDL ppb
SRM Full-scan
150 compounds in mixed vegetable matrix (QuEChERS)
Triple quadrupole level sensitivity possible with a non-target acquisition *Acquired on the Q Exactive GC system – the Exactive GC system provides equivalent performance
Pesticide Residues
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LOD/LOI
Limits of detection and identification in fruit and vegetable matrices
Pesticide Residues
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Pesticide residues
Pesticide Residues
“The overall outcome of the evaluation is that GC-EI-full scan Orbitrap HRMS is considered highly suited for pesticide residue analysis. With that, it provides an alternative to GC-triple quadrupole MS, with the advantage that the measurement is more straightforward, and that besides quantitative determination an additional screening can be performed for other analytes.”
H.G.J. Mol, M. Tienstra, P. Zomer, Evaluation of gas chromatography -electron ionization - full scan high resolution Orbitrap mass spectrometry for pesticide residue analysis, Analytica Chimica Acta (2016)
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Pesticide residues
Pesticide Residues
“These good results present the advantages derived from full scan analysis applicable to other compounds not present in the selected and retrospective evaluation together with an easier scope management compared with GC-TQ-MS/MS.”
Ucles, S., A., Lozano, A., M.J. Mart´inez Bueno, Fernandez-Alba A.R. SHIFTING THE PARADIGM IN GAS CHROMATOGRAPHY MASS SPECTROMETRY PESTICIDE ANALYSIS USING HIGH RESOLUTION ACCURATE MASS SPECTROMETRY, Journal of Chromatography A (2017)
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Chlorinated paraffins
Persistent Organic
Pollutants
• Currently there is no consensus for the use of a validated analytical procedure for routine monitoring of CPs in food and feed.
• SCCPs and MCCPs have thousands of homologues and isomers that cannot be separated chromatographically.
• This, together with low concentrations makes their detection and quantification difficult.
0 2 4 6 8 10 12 14 16
Time (min)
0
10
20
30
40
50
60
70
80
90
100
Rel
ativ
e A
bund
ance
10.07
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High resolution accurate mass selectivity 63% C10-C13 technical mix, NCI, 60k resolution
C10H15Cl6
C11H17Cl6
10.15
C11H16Cl7
10.73
C12H18Cl7
10.69
11.21
10.22
11.70
9.72
RT: 6.48 - 14.43
6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 Time (min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
Rel
ativ
e A
bund
ance
NL: 2.00E8 TIC MS
NL: 2.00E7 m/z= 346.92652
NL: 3.00E7 m/z= 360.94208
NL: 3.00E7 m/z= 394.90330
NL: 2.00E7 m/z= 408.91872
NL: 2.00E7 m/z= 444.87597
NL: 2.00E7 m/z= 458.89157
NL: 2.00E7 m/z= 492.85283
TIC
11.20
C12H17Cl8
11.73 C13H19Cl8
C13H18Cl9
Persistent Organic
Pollutants
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Negative chemical ionization: Linearity for SCCP 63% C10
y = 1906.6x - 122811 R² = 0.9998
y = 11063x - 293814 R² = 0.9998
y = 10121x - 385111 R² = 0.9997
y = 2948.3x - 195135 R² = 0.9996
0.00E+00
1.00E+07
2.00E+07
3.00E+07
4.00E+07
5.00E+07
6.00E+07
0 1000 2000 3000 4000 5000 6000
peak
are
a co
unts
Concentration [pg/µL]
m/z 312.9665
m/z 346.9275
m/z 380.8886
m/z 416.8466
Excellent compound linearity (25-5,000 ppb) was obtained for these C10 chlorinated homologues present in the SCCP 63% technical mixture.
Persistent Organic
Pollutants
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Chlorinated parafifns
Persistent Organic
Pollutants
“Using high resolution, accurate mass Orbitrap-MS enables much deeper insights into the pattern and content of CPs without having to fear mass interferences from other CPs or halogenated compounds such as PCBs. Preliminary results suggest that determination of both CPs and PCBs in the same sample in one run is possible, representing a potential for shorter sample preparation and quicker analyses of these types of POPs in food.”
HIGH RESOLUTION ACCURATE MASS SCREENING FOR CHLORINATED PARAFFINS IN FOOD SAMPLES USING GC-ORBITRAP MASS SPECTROMETRY (Kerstin Krätschmer et al. Dioxin 2017)
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Polybrominated diphenyl ethers
Persistent Organic
Pollutants
• European guidelines stipulate extremely low concentrations
• Analytical methods with a limit of quantification of 0,01 ng/g wet weight or lower
• BDE 209 (decabromo) limit is 10 ppt in the sample
x=1-5, y=0-5
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Tuna sample spiked 0.01 ng/g PBDEs
Persistent Organic
Pollutants
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Polybrominated diphenyl ethers
Persistent Organic
Pollutants
“GC-Orbitrap is a useful tool for control labs,
outstanding sensitivity…high selectivity when
analyzing complex matrices…high robustness
…helps to fulfill new regulations with
extremely low limits (e.g. PCBs, PBDEs).”
Practical Experiences of Implementing POPs Methods using Orbitrap™ GC-MS. Nuria Cortés-Francisco, BFR 2017
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Food contact materials
Full MS [50-550 Da]
NIST C31H52O3 472.3907 m/z
α-Tocopherol acetate
HRF values > 95
Food Contact Materials
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Food contact materials
Food Contact Materials
Full MS [50-550 Da]
NIST
165.0909
472.3907
430.3801 C29H50O2 C10H13O2
430.3805 165.0910
165.0909 430.3801
0.109 0.871
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Food contact materials
Food Contact Materials
PRECURSOR ION FRAGMENT IONS
Rt Accurate
mass value (m/z)
Formula Proposed SI* Score
* HRF
*
Accurate mass value
(m/z)
Formula proposed
Mass Deviation* (ppm/mDa)
Identified compounds
9.8 300.1567 C15H24O6
827 96.6 98.0 113.0597 55.0178
C6H9O2 C3H3O
1.4 / 0.2 1.6 / 0.1
tripropylene glycol diacrylate
11.0 294.3281 C21H42
820 96.4 99.0 69.0699 83.0855
C5H9 C6H11
0.5 / 0.03 0.3 / 0.02
10-Heneicosene
29.6 472.3911 C31H52O3
898 97.5 99.8 430.3801 165.0909
C29H50O2 C10H13O2
0.9 / 0.4 0.8 / 0.1
alpha-Tocopherol acetate
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Food contact materials
Food Contact Materials
“HRAMS has shown to be a useful analytical approach for the elucidation of NIAS based on the accurate mass measurement in full scan and fragmentation modes using the Q-Orbitrap-MS analyser. the combination of accurate mass matching and explaining the ions observed in the spectrum provides a fast and confident route to the identification of unknown compounds.”
Identification of non-intentionally added substances in food packaging nano films by gas and liquid chromatography coupled to Orbitrap mass spectrometry M.J. Martínez-Bueno, M.D. Hernando, S. Uclés, L. Rajski, S. Cimminoc, A.R. Fernández-Alba: Talanta 172 (2017) 68–77
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Whiskey authenticity
Single distillery
Bourbon 3 wood aged
Pool
PCA : Bourbon and 3 wood aged clearly different from other whiskies. Single distillery whiskies also show clear differences.
10 year
15 year
15 year
Authenticity
Trans-β-ionone
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Whiskey authenticity
Authenticity
Authenticity “GC coupled with Orbitrap MS is a major step forward…Q Exactive GC provides a comprehensive chemical profile of a sample, detecting both major and minor components with a high degree of confidence (spectral quality and linearity)…Sophisticated, yet simple to use, software tools provides fast isolation of peaks of interest and intelligent compound identification with sub 1 ppm mass accuracy.”
Professor Jana Hajslova, Jana Pulkrabova, Michal Stupák – RAFA 2016
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The impact of Orbitrap GC-MS in food analysis
Orbitrap HRAM Mass
Spectrometry Pesticide Residues
Authenticity Food Contact Materials
Persistent Organic Pollutants
• Considered highly suited for pesticide residue analysis
• Alternative to GC-triple quadrupole MS systems
• More straightforward, • Easier scope management
• a fast and confident route to the identification of unknown compounds
• enables much deeper insights without having to fear mass interferences
• a potential for shorter sample preparation and quicker analyses
• outstanding sensitivity • high selectivity • high robustness
• a major step forward • comprehensive chemical
profile • high degree of confidence • simple to use, software
tools • intelligent compound
identification
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