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GC/MS-Komplettlsungen von Agilent. Der schnellste Wegzur sicheren Methoden-Implementierung fr Ihr Labor
GC MS Euro Tour 2011Page 1
Bernhard Rothweiler
Senior Applications Chemist
Europe, Middle East, Africaand India
New technologies essential to
meet higher productivity needs but
Requires time for startup
Requires high investigation costs
May generate questionable results
GC MS Euro Tour 2011Page 2
May generate questionable results
Agilent Analyzer:
Get on a fast track to higher productivity
What is different when ordering an Analyzer?
CheckoutSystem with
#SP1: Factory setup and tested analyzer
Familiarization
Customer CD
Customer CD
w/o Analyzer
GC MS Euro Tour 2011Page 3
IndividualComponents
produced
IndividualComponentsTested (OFN)
Systemassembled
App. methoddeveloped oncust. system
Systemcheckout on
App. mix
Run 1st
customersample
customizationor optimization
method
On-goingmaintains and
service
Factory CE Setup; I&F Optional Consulting After InstallationWithout Ordering Analyzer
Factory Setup
Optional
Consulting After InstallationOrder Fast Track Analyzer
CE Specialist
I&F
reportapplication setup & consultingApp. optimized
consumablesStd. HW, SW
http://www.agilent.com/about/newsroom/lsca/imagelibrary/images/lsca_98.jpghttp://www.sisweb.com/art/sge/gccol.jpg
No More Struggle for DevelopingMethods
Sampleready
OrderStandardcheckout
Standardfamiliarization
GC MS Euro Tour 2011Page 4
Agilent developsmethod
Orderkit
Applicationcheckout
Applicationfamiliarization
RefinemethodOrder
Universal methods to startup application , meeting most testing needs!
Analyzers are flexible, can be adapted to customer needs
MSD Analyzer
Pesticide
GC/MSD Analyzer ( Backflush, MMI, DRS, Pesticide library)
GC/MSD Analyzer ( Backflush, MMI, DRS, Jap. List Pesticide library)
GC/MSD Analyzer ( Backflush, MMI, FPD, ECD, DRS, Pesticide library)
Forensics2 Toxicology Screening GC-MS Analyzer
GC MS Euro Tour 2011Page 5
2 Toxicology Screening GC-MS Analyzer
Backflush, MMI, SIM/Scan/NPD, DRS, Forensic/Tox library
Backflush, S/S inlet, SIM/Scan, DRS, Forensic/Tox library
VOCs
HSS/GC/MSD Analyzer ( S/S or MMI, SIM/Scan, DRS, Solvents+ library)
PAHs
GC/MSD Analyzer ( Backflush, MMI, DB-EUPAH column )
926 Pesticide Analyzer
Factory All checkout on your system System setup and instrument leak tested Application appropriate column, liner and septa pre-installed Retention time locked on your instrument Capillary flow device setup for backflushing DRS, AMDIS & NIST & RTL Pesticide libraries installed Run pesticide checkout mix perform DRS analysis Signal/Noise check
Delivery Quick start guide for checkout method
GC/MS Pesticide Analyzer
GC MS Euro Tour 2011Page 6
Deliverywith EasyTools
Quick start guide for checkout method All factory checkout results on CD ROM Training videos Consumables included, no separate ordering required Trial SPE QuEChERS kits (AOAC and EN methods) Easy consumables re-ordering information
ApplicationfocusedInstallation
Agilent CE makes sure you are ready to runreal samples before he/she leaves
State-of-the-Art Technologies to Improve
Pesticides Screening with Agilent GC/MSDAnalyzer
Deconvolution
Reporting SW (DRS)
Retention Time
Locking (RTL)
Capillary Flow
Technology (CFT)
GC MS Euro Tour 2011Page 7
RTL databases
for 926 pesticide compounds
App. specific consumables
Sample Prep. QuEChERs
Multi-Mode Inlet,
SIM/SCAN; QEdit
Agilent Pesticide Analyzer:
Data File:
Adjacent Peak Subtraction = 1
Resolution = Medium
Sensitivity = Medium
MSD Deconvolution
Sample Name: carrot1 to here in 2 - 3 min
from here
Screen for 926
GC MS Euro Tour 2011Page 8
Chem R.T. Diff
station sec.
4.4196 33704619 Cashmeran 13.59 60 13.1 67 35
6.9401 1517222 Phenanthrene-d10 35.96 24.68 92 9.2 79 2
8.0245 84695 Diisobutyl phthalate 16.19 9.88 83 9.2 81 9
9.27 84742 Di-n-butylphthalate 61.5 23.38 95 7.5 92 1
12.136 72559 p,p'-DDE 6.15 3.52 87 15 82 1
12.9476 72548 p,p'-DDD 2.6 1.55 69 12.5 77 5
12.954 789026 o,p'-DDT 2.6
13.5916 50293 p,p'-DDT 2.85 1.33 70 12 71 3
13.9963 115866 Triphenyl phosphate 15.11 9.18 95 16.1 84 1
14.9048 117817 Bis(2-ethylhexyl)phthalate 4.46 56 9.6 64 62
14.99 2385855 Mirex 1.38
6.943 Phenanthrene-d10 10
Data File:
Date/Time: 2:45:59 PM Thursday, February 19, 2009
Sensitivity = Medium
Shape Requirements = Medium
Match Reverse
Match
Hit
Num.
The NIST library was searched for the components that
R.T. Cas # Compound Name AMDIS
Amount (ng) AMDIS NIST
Screen for 926
pesticides in
one 21-minute
GC/MS run
50
170 280
31075
185
160
How Does Deconvolution Work?
GC MS Euro Tour 2011Page 9
Extracted IonChromatograms
(EIC)
After de-skewing
50
170
280
75 late retention time185 shape & early retention time
310 early retention time
160 shape
same shape and sameretention time
AMDIS Deconvolution Pulls Out IndividualComponents and their Spectra
Deconvoluted components and spectra
matrixTIC
Component 1
Component 2
Component 3
Components and MixedSpectra
GC MS Euro Tour 2011Page 10
target
interferenceComponent 3
Deconvolution
Rawspectrum
Deconvolutedspectrum
GC MS Euro Tour 2011Page 11
spectrum
Libraryspectrum
p,p-DDE
DRS Report from 3 Integrated Processes
Total ion chromatogram
Targets are identified byDeconvoluted Target
AMDIS deconvolutescomponent spectra and
GC MS Euro Tour 2011Page 12
Combined quantitative and qualitative
HTML summary report
Quant Results
Targets are identified bycomparison to locked R.T.sand 3 qualifier ion ratios,then quantified using targetion area vs ISTD cal table
Deconvoluted Targetspectra confirmed byAMDIS, searched againstNIST08 MS database
Confirmed NIST08 hits
component spectra andsearches target MS databaseusing locked RT as a qualifier
Confirmed AMDIS hits
AMDIS Quant Result
Spinach Report, results from 3 DRS processes
NIST 08 Match and Hitnumber of the top 100hits from 191,000+compounds
GC MS Euro Tour 2011Page 13
ISTD, used for targets amount
Match against
AMDIS library
RT diff in sec. vsexpected locked RT
Configuration of New Tox AnalyzerPost column Capillary Flow Technology (PUU) device provides:
A) BackflushingB) No vent column changingC) Overpressure protection
LiquidInjector
AUX EPC
2.73 psig
VentPurged Ultimate
Union (PUU)
GC MS Euro Tour 2011Page 14
7890AGC
S/S Inlet
Column
15 m X 0.25 mm id X 0.25 um DB-5MSUI
5975CMSD
Diffusion
(or Turbo)
1m x 0.15 mm id
PUU
Real Blood Extract From Tox Lab.
Scan
GC MS Euro Tour 2011Page 15
SIM
DRS Report From Blood Sample
AMDIS is used for compound identification. ChemStation is usedfor quantitative measurement of compound.
GC MS Euro Tour 2011Page 16
GC/MS/MS Analyzer
GC MS Euro Tour 2011Page 17
MS1 Quad andPost Filter
CollisionCell
Pre Filter and MS2Quad
DetectorSource
7000 B MS/MS SystemOptimized for gas chromatography
MS/MS Ensures Lowest Detection LimitsEI: spectrum of analyte can also includeions from matrix, column bleed, gases, etc.
Product 1
Product 2
GC MS Euro Tour 2011Page 18
Q1 SIMisolate precursorbefore CID
Product 1Product 3
CID +
Q2 SIM
Lower m/z ProductIons measured againstzero chemical noise
chemical noisefrom these otherions is eliminated
MS/MS Ensures Highest Selectivity
Pike Extract
GC MS Euro Tour 2011Page 19
Apple
Cabbage
SIM - EIC (246) MRM (2 transitions)
S/N = 448
S/N = 241
Consistent, High Quality ResultsSIM versus MS/MS Comparison: Food Safety
GC MS Euro Tour 2011Page 20
Orange
Spinach
Ginseng
S/N = 456
S/N = 260
S/N = 446
State-of-the-Art Technologies to ImprovePesticides Analysis with Agilent
GC/MS/MS Analyzer
Dynamic MRMRetention Time
Locking (RTL)
Capillary Flow
Device for Backflushing
GC MS Euro Tour 2011Page 21
MRM DB for 500+Pesticides
Locking (RTL)
App. specificconsumables
Sample Prep.QuEChERS
Multi-Mode Inlet,
Cold Splitless
SP1 Pesticide Analyzer MRM Methods
7890-0501 7890-0502
setup post-column BF mid-column BF
flow control constant pressure constant flow
# of Analytes in DB 500+ 200+
# of Analytes in method 200+ 200+
GC MS Eu
