GC/MS-Komplettlösungen von Agilent. Der schnellste Weg .GC/MS-Komplettlösungen von Agilent. Der

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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