5977A SQ 5977E SQ 5975T LTM SQ Agilent GC/MS More Choices ... · The precursor ion should NOT be...
Transcript of 5977A SQ 5977E SQ 5975T LTM SQ Agilent GC/MS More Choices ... · The precursor ion should NOT be...
240 IT 7890 GC 7000 TQ
7890 GC
5977E SQ 7820 GC
5975T LTM SQ
5977A SQ 7890B GC
7200 Q-TOF 7890GC
More Choices – Better Solutions
Agilent GC/MS/MS
Agilent GC/MS
Basic Questions – Which GC/MS Solution?
Target analysis Clean Matrix
SQ, IT, Q-TOF Scan with libraries
QqQ in SQ mode Scan with library Search
SQ SIM with ion ratios
QqQ, IT, Q-TOF MS/MS with ion ratios
Unknowns Analysis Clean Matrix SQ, IT, Q-TOF Scan with libraries
QqQ in SQ mode with library Search
Q-TOF Accurate Mass with Formula calculator
IT, Q-TOF CI for Molecular Weight
IT, Q-TOF MSMS product ion scan
Basic Questions – Which GC/MS Solution?
Target analysis in Matrix
SQ SIM with Ion Ratios
SQ Deconvolution – RTL – RTL Libraries
QqQ, IT, Q-TOF MS/MS with ion ratios
IT, Q-TOF CI for Molecular Weight
Q-TOF Accurate Mass with narrow extraction window
Unknowns Analysis in Matrix SQ, IT Deconvolution – RTL – RTL Libraries
QqQ in SQ mode Deconvolution – RTL – RTL
Libraries
Q-TOF Accurate Mass with Formula calculator
IT, Q-TOF CI for Molecular Weight
IT, Q-TOF MSMS product ion scan
New Agilent 5977 Series GC/MSD
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What is the same as 5975? Quality
Reliability
Proven core technology since 5973/5975
• Inert Ion Source
• Heatable Gold Quartz Quadrupole
• Triple Axis Detector
Trace Ion Detection
Gain Normalized Methods
Retention Time Locking
New Agilent 5977 Series GC/MSD
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• Improved Sensitivity with Extractor Ion Source
• Improved Asset Utilization
• MassHunter GC/MS Acquisition – Looks like Chemstation
• MassHunter and MSD ChemStation data analysis
• Integration of new Agilent Vacuum Pumps brings intelligent
operation
• Green Technology – Energy and Gas Savings
Inert Flow Path
Improved Performance - Deliver better results
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UltiMetal – TCD,
FPD, NPD/FID Jets
UltiMetal Capillary Flow Technology
Devices, Ultimate Union
UltiMetal Inlet Weldment, Shell
and Transfer Lines
Ultra Inert GC Column
Ultra Inert Gold Seal
Ultra Inert Inlet
Liner
New UltiMetal
FlexiMetal Ferrules
Technical …now from a single supplier
Extractor Source “Etune” Sensitivity Increase
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Blue – Extractor 40ppb solution (SVOC)
Red – Standard 40ppb solution (SVOC)
Agilent 7000 B GC/MS/MS Advantages
Used For • Target Analysis in Complex Matrices
Superior Results • Improved compound identification - MS/MS for matrix elimination
• Lower detection limits
• Lower rsds - Dynamic MRM – more segments
= longer dwell time per analyte
Increased Sample Thruput • Shorten run time using MS separation
• Backflush – Save bakeout time at end of run
• LTM – Low Thermal Mass Technology –
GC x GC with fast temperature ramping
Operator Time Savings •Batch processing/review
•MRM Libraries and DynamicMRM – Faster method development
Why MS/MS?
Greater Selectivity Than SIM
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Precursor
Ion
Product 1 Product 3
Product 2
EI-SIM selectivity proportional to
spectral resolution
no selectivity against ions
with same m/z
EI-MS/MS Precursor selectivity same as SIM
High probability that at least one product
ion will be a unique dissociation product
of the precursor BUT not the interference interference
analyte
interference
The precursor ion should NOT be used for ion
ratios or quantitation since the interferences will
be the same as the SIM ion
unit mass resolution
Oct
obe
r,
201
0
Advantages of a QQQ as a Chromatographic
Detector - Multiple Reaction Monitoring (MRM)
170 210 250 290
210
222
268 280 165
Spectrum with
background
ions (from EI)
Q1 lets only
target ion 210
pass through
190 210
210
Collision cell
breaks ion 210
apart
150 170 190 210
210 158
191
Q2 monitors
fragments 158
and 191 for quant
and qual.
160
158
190
191
no chemical background
Quad Mass Filter (Q2) Quad Mass Filter (Q1) Collision Cell Source
Average and exact Molecular Weight
Each compound is classified in two categories
Database has RTs (and RIs) to be used with three GC methods (CF-40min, CP-40min, and CF-20min)
G9250AA – Pesticide / Environmental Pollutant MRM Database
The Flexibility: Multi-transitions; classifications; 3 RTs and RIs
QqQ MS/MS For Multiple Compounds in Matrix
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240 Ion Trap
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Used For • Target and Unknowns Analysis - Flexibility
Superior Results • Improved compound identification - MS/MS for matrix elimination
• Chemical Ionization for molecular weight information
• Lower detection limits in matrix
Increased Sample Thruput • Shorten run time using MS separation
• Backflush – Save bakeout time at end of run
Operator Time Savings •Batch processing/review
Internal Ionization Flexibility
EI Full-
scan CI Full-
scan
CI /MS/MS
EI /MS/MS
EI/ SIS
EI Full-scan
Agilent 7200 TOF / QTOF For Unknowns
Accurate Mass Full Scan for Matrix Elimination
• Narrow mass window filters out matrix interference
• High acquisition speeds – for superior deconvolution
• Future Data Mining
• Sensitive
• 5 orders of dynamic range
Accurate Mass for Unknowns/Non-Target Identification
• Accurate mass with good mass resolution
• High isotope ratio fidelity
• Formula Calculator
• Molecular Structure Correlator
• NIST compatible
• ChemSpyder – Free Structural Database
Resolving power & mass accuracy
R = 614/0.68 = 903
Δmz = 0.1/614
= 160 ppm
Pw=0.68
Mz=614
SQ
TQ
IT
TOF
Q-TOF
R = 614/0.0423 = 14522
Δmz = 0.0004/613.96
= 0.7 ppm
Resolving Power:
R=mz/PWHM
Mass Accuracy: Δmz=dm/mz*106,
parts per million (ppm)
PFTBA mass 614
C12F24N=613.964203
1 Da.
1 Da.
Many possible formulas with an MSD or IT But only a few with TOF
1
10
100
1000
10000
0.1 1 10 100 1000
# P
oss
ible
Ch
emic
al F
orm
ula
s
mass uncertainty, ppm
Possible Number of Chemical Formulas at m/z 272
Formulas made of:
C,H,N,O,F, & Cl
mass uncertainty
ppm amu # of Possible
Formulas 1000 0.3 7657
368 0.1 4050 100 0.03 1223
37 0.01 466 10 0.003 120
4 0.001 43 1 0.0003 11
0.4 0.0001 5 0.1 0.00003 2
Octafluoronaphthalene (CAS
313-72-4)
C10F8 = 271.98667
Accurate mass reduces risk of investing effort on the wrong molecule
Okra QuEChERS Extract
Matrix interferant ion (b-Tocopherol)
150.06839 Da
Analyte Indoxacarb ion (100pg)
150.01195 Da (fragment ion)
Dm = 0.05644 Da.
Extraction window
+/-0.5 amu (~ 300ppm)
Indoxacarb b-Tocopherol
Indoxacarb
TOF Accurate Mass to Eliminate Matrix Interferants
Tocopherol
interference
eliminated in
MS mode
If even more selectivity is needed, option of MS/MS
MS/MS with high resolution and accurate mass!
Extraction window
+/-0.010 amu (~ 6ppm)
TIC and EICs of Coffee Extract
2-formyl thiophene
m/z 111.9983 ± 100 ppm
2-acetyl thiazole
m/z 127.0092 ± 100 ppm
GC/MSD Software
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MassHunter Qual
MassHunter Quant MH
CS
MassHunter GC/MS Acquisition
And Use Either
MassHunter Data Analysis
OR
MSD ChemStation Data Analysis MSD ChemStation DA
G1701FA
Batch-at-a-Glance Batch Table: Single Compound/Multiple Compounds
Single Compound, Qualifier, ISTD, ISTD Qualifier
Multiple Compounds
Batch-at-a-Glance Powerful Navigation
Outlier Detection
39 Outlier Criteria
Limits in method
Flagging &
Filtering
Outlier Report
Excel-based Reporting Powerful Reporting using Excel + XML
Choose Report Template
Queue up Multiple Reports
Choose Printer, PDF
Excel is launched
Template is loaded
Results are imported
Report is formatted
Report is:
a) saved as XLS
b) OPT: send to Printer
c) OPT: saved as PDF
Report Results (XML) &
Graphics are generated
Thank You
May 13, 2013
Confidentiality Label
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