agilent’s gc/ms & gc/ms/ms analyzers for environmental labs · pdf...

Agilent’s GC/MS & GC/MS/MS Analyzers for Environmental Labs

Philip L. Wylie, Ph.D.

Agilent Technologies

Wilmington, DE

Users Meeting: Tucson March 2014

[email protected]

Today’s Challenges Expecting More from Less

• Increasing cost of ownership

• Trace analysis in complex matrices

Business Challenges

• Less time for method development

• Limited technical experience

Resource Allocation

• Demands for higher throughput

• Quicker return on capital investment

Optimizing Efficiency

2 September 2013 MS Analyzer Overview

Typical Approach to New Method Implementation

Order all the parts

…Test and validate the new method

Find or develop

the method

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http://images.google.com/imgres?imgurl=http://www.freeclipartpictures.com/clipart/clip-art/pictures/carrots.jpg&imgrefurl=http://www.freeclipartpictures.com/clipart/food70.htm&usg=__QWKhmDfN77iipfV-EdeXfSY8uHI=&h=768&w=1024&sz=80&hl=en&start=6&tbnid=2bV24H2q2JULaM:&tbnh=113&tbnw=150&prev=/images?q=carrots&imgsz=xxlarge&gbv=2&hl=en

http://images.google.com/imgres?imgurl=http://mwlfood.files.wordpress.com/2008/12/raw-whole-zucchini.jpg&imgrefurl=http://mwlfood.wordpress.com/2008/12/14/516/&usg=__lCRMtzQiME8YOQrNMLYe9MmBRl4=&h=795&w=1439&sz=114&hl=en&start=5&tbnid=guswsOpTgm7bZM:&tbnh=83&tbnw=150&prev=/images?q=zucchini&imgsz=xxlarge&gbv=2&hl=en

http://images.google.com/imgres?imgurl=http://www.nitamin.com/images/potatoes.jpg&imgrefurl=http://beansgotgas.blogspot.com/2007/08/hello-everybody.html&usg=__pVGqNsVSkIH-5w7XbQrmFolPS0E=&h=1024&w=1280&sz=802&hl=en&start=1&tbnid=2b1Uw0si3PAbrM:&tbnh=120&tbnw=150&prev=/images?q=potatoes&imgsz=xxlarge&gbv=2&hl=en

http://images.google.com/imgres?imgurl=http://www.nutritionresearchcenter.org/healthupdate/uploaded_images/Grapes-753654.jpg&imgrefurl=http://www.nutritionresearchcenter.org/healthupdate/labels/cancer.html&usg=__H3AH1dzX2f3lwl5qFTXwodm43BM=&h=768&w=1024&sz=182&hl=en&start=2&tbnid=BrdMre0Lm1c9RM:&tbnh=113&tbnw=150&prev=/images?q=grapes&imgsz=xxlarge&gbv=2&hl=en

http://images.google.com/imgres?imgurl=http://blogs.phillyburbs.com/news/intelligencer/wp-content/blogs.dir/4/files/Kennedy/tomatoes1024.jpg&imgrefurl=http://blogs.phillyburbs.com/news/intelligencer/you-say-tomato-i-say/&usg=__vzP50v9oz3HtVLYOQaFWf63Vjmk=&h=769&w=1024&sz=151&hl=en&start=1&tbnid=wy3R4uSw21wsIM:&tbnh=113&tbnw=150&prev=/images?q=tomatoes&imgsz=xxlarge&gbv=2&hl=en

http://images.google.com/imgres?imgurl=http://www.moograssfarms.com/images/Strip-steak-MCB-MaggieO.jpg&imgrefurl=http://www.moograssfarms.com/index.php?cPath=21&osCsid=a01a2550b1311eea243f5697fb7c5dbe&usg=__BGe1lFM9dwQnZ2vVQm_n7x_cLTQ=&h=768&w=1024&sz=491&hl=en&start=1&tbnid=634cyQJm81cHhM:&tbnh=113&tbnw=150&prev=/images?q=raw+steak&imgsz=xxlarge&gbv=2&hl=en

Agilent analyzers arrive ready to use!

You’ll be running real samples

before the service engineer

leaves your lab

Why spend more $ to buy an analyzer?

Background: A major Chinese independent lab required a single injection

GC/MS/MS method to analyze 323 pesticides in vegetables

Instrument

Time for method

development

Chemicals

Required End Result

Other Vendor’s

System 32 weeks of hard work

323 chemical

standards

Poor results, not happy,

switched to Agilent

Agilent Pesticide

Analyzer 1.0

2 weeks, to add cmpds

and adjust method

34 compounds

not in 0501 Database Happy!

Agilent Pesticide

Analyzer 2.0

3 minutes

(NOT weeks, NOT days,

NOT hours)

None Love it !!!

Agilent Pesticide

Analyzer 3.0

(Coming May 2014)

Contains 5 GC/QQQ

Methods (2 new 20-min

methods)

None It’s even easier to use!

To build the database Agilent performed >3000 runs, so you don’t have to!

5 ASTS 2012

App. optimized

consumables

Pre-Configured Analyzers Increasing Your Productivity

Application

report

System with

application setup

w/o Analyzer

Familiarization

Common

Components Factory Configured with Chemical Testing

Field Verification

Std. HW, SW Customer

Configured Analyzer Solution

You can focus on analyses - not method development!


http://www.agilent.com/about/newsroom/lsca/imagelibrary/images/lsca_98.jpg

http://www.sisweb.com/art/sge/gccol.jpg

GC/MS Analyzers Relevant to Environmental Analysis

Analyzer

Us

es

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S

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Pre

-

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talle

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# A

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lyte

s

• Pesticide Analyzer Yes Yes Yes Yes Yes *927

• Greenhouse Gas & Soil Gas Analyzer

• CH4, N2O, CO2, (O2, N2,SF6)

• 6 versions depending on analytes &

concentrations

No Yes Yes Yes Yes

3

5

or

6

• Semivolatiles Analyzer Yes Yes Yes Yes Yes *338

• 3-in-1 Environmental Analyzer

• VOAs, Semi-VOAs & Pesticides Yes Yes Yes Yes Yes

*369

*338

*927

• Enhanced PAH Analyzer with H2 bleed No Yes Yes Yes Yes 29

• Volatiles Analyzer Yes Yes Yes Yes Yes 63

*(369)

* Number of compounds in the DRS database/library

GC/QQQ Analyzers Relevant to Environmental Analysis

Analyzer

Rete

nti

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oc

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Us

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flu

sh

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Fa

cto

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Ch

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Co

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# A

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• Pesticide & Environmental Pollutants Analyzer Yes Yes Yes Yes 1074

• Enhanced PAH Analyzer

• H2 bleed gives linear calibrations & response

stability

Yes Yes Yes Yes 30

*(338)

* Comes with the semivolatiles library that includes PAHs

Agilent’s DRS Analyzers

• GC/MS analyzers pre-configured and chemically tested for analysis to ensure optimal performance of your instrument and application.

• Optimized analyzer includes GC column, consumables, calibration/checkout samples, and analytical method to reduce the time you spend configuring individual components.

• Integrated Capillary Flow Technology backflush for a more robust analysis while reducing run time and system maintenance.

• Includes CD-ROM with optimized retention time locked acquisition method for your analytes, a DRS database, application note, and quick start guide for faster method development.

• On-site installation and check out of the GC/MS Analyzer by a factory certified technician confirms that your instrument and application meet Agilent’s analytical performance criteria.

• System familiarization ensures that your team is “ready to go” with calibration and validation immediately following system installation.

March 24, 2014

Confidentiality Label

9

Let’s Focus on Three Analyzers

March 24, 2014


10

DRS Pesticides Analyzer (GC/MS)

Enhanced PAH Analyzer (GC/MS/MS)

Pesticides and Environmental Pollutants Analyzer (GC/MS/MS)

GC/MSD DRS Analyzers – What they can do.

From here…

…to here in 2 - 3 min

RTL Pesticide Databases

Deconvolution Reporting Software

QEdit

Quant on Normal or

Deconvoluted Peaks

GC/MSD in Scan Mode

DRS Report from 3 Integrated Processes

Total ion chromatogram

Combined quantitative and qualitative HTML

Summary report

Quant Results

Targets are identified by

comparison to locked R.T.s

and 3 qualifier ion ratios,

then quantified using target

ion area vs ISTD cal table

Deconvoluted target spectra

confirmed by AMDIS are

searched against NIST08 MS

database

Confirmed NIST08 hits

AMDIS deconvolutes

component spectra and

searches target MS database

using locked RT as a qualifier

Confirmed AMDIS hits

AMDIS Quant Result

AMDIS Deconvolution Pulls Out Individual Components and their Spectra

TIC & Spectrum

TIC Sum of ions in Component 1

Sum of ions in Component 3

Sum of ions in Component 2 Decon

volu

tion

Deconvoluted peaks and spectra

Metalaxyl Identified by DRS in Mixed Vegetable (QuEChERS) Extract (AMDIS View)

TIC

Spectrum before

Deconvolution

Deconvoluted spectrum (white)

and library spectrum (black)

Metalaxyl burried

in matrix

DRS Report for Spinach Extract after importing AMDIS Results, QEdit reviewed with manual integrations

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00

TICs of Surface Water Extracts

How many pesticides

(drugs, allergens etc.) are in

these samples and how long

does it take you to confirm?

17 Surface Water TICs (Scan): Pesticide Analysis Using DRS with Agilent Pesticide Database (927 entries)

*CDFA is the California Department of Food and Agriculture Data files courtesy of Dr. Mark Lee and Steve Siegel

CDFA* Agilent DRS

Targets Found

(not counting ISTD) 37

Same 37

+99 more

False Positives 1 0

Processing Time ~8 hrs

(ChemStation Only) 25 min

Agilent has solved all the typical PAH analysis problems!

March 24, 2014


18




Enhanced PAH Analysis GC/MS/MS Analyzers

• Hydrogen bleed to clean source

• MRM database including optimized transitions

for 350+ environmental pollutants (PCBs, PAHs

and semi-volatile compounds)

• Retention Time Locked application-specific

column

• Multimode inlet for large volume injection helps

optimize detection limit performance

• Capillary Flow Technology Backflush for faster

cycle time and reduced system maintenance

• PAH MRM acquisition method, quick start

guide, and Application Note that show you how

to set up the analysis method provided with the

Analyzer

• CD-ROM with factory checkout results, data

files, and reports

GC/MS/MS PAH Analyzer

19 September 2013

MS Analyzer Overview

PAH Analysis

March 24, 2014 Confidentiality Label

20

4.00 6.00 8.00 10.00 12.00 14.00 16.00

4

3 5,6,7

9

10

12

11

13

14

1,2

17 18

20 21

22,23

25,26,27

2

4

28,29

31

32,33

15,16 30

34

Internal Std 4 2-Methylnaphthalene 15 Phenanthrene 26 Benzo[k]fluoranthene

1 Naphthalene-d8 5 Biphenyl 16 Anthracene 27 Benzo[j]fluoranthene

9 Acenaphthene-d10 6 2,6-dimethylnaphthalene 17 1-methylphenanthrene 28 Benzo[e]pyrene

14 Phenanthrene-d10 7 HMB 18 Fluoranthene 29 Benzo[a]pyrene

24 Benzo[a]pyrene-d12 8 Acenaphthylene 20 Pyrene 30 Perylene

10 Acenaphthene 21 Benz[a]anthracene 31 Dibenz[a,c]anthracene

Target Compounds 11 2,3,5-trimethylnaphtha... 22 Triphenylene 32 Dibenz[a,h]anthracene

2 Naphthalene 12 Fluorene 23 Chrysene 33 Indeno[1,2,3-cd]pyrene

3 1-methylnaphthalene 13 Dibenzothiophene 25 Benzo[b]fluoranthene 34 Benzo[ghi]perylene

NOAA 29 PAHs: GC/MS with Constant Flow Backflush GC/MS Analyzer

GC/MSD PAH Analyzer

Self-Cleaning Ion Source In situ or on-board source cleaning

Hydrogen fed in via

transfer line

Hydrogen flows concentrically

around end of column into the

MSD ion volume. Repeller

Draw out /

Extractor lens

Enhanced PAH and P&EP Analyzer Intro

21 August 2013

Automated Offline Source Cleaning

7890B

GC

Conditions: 0.4 mL/min, Source 350°C, Filament On

Liquid Injector

Column 5977A MSD

or

7000B

MS/MS

S/S Inlet

Helium

Self Cleaning Control Module

He Carrier Gas

H2 0.4 mL/min

Source


22 August 2013

Self-Cleaning Ion Source Using H2 to Clean to MS Source

5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0 5 0 0

0

5 0 0 0

1 0 0 0 0

1 5 0 0 0

2 0 0 0 0

2 5 0 0 0

3 0 0 0 0

3 5 0 0 0

4 0 0 0 0

4 5 0 0 0

5 0 0 0 0

5 5 0 0 0

6 0 0 0 0

6 5 0 0 0

7 0 0 0 0

7 5 0 0 0

m / z - - >

A b u n d a n c e

A v e r a g e o f 1 . 9 6 9 t o 1 0 . 0 4 6 m i n . : E I - b a c k g r d - r e p 0 . D \ d a t a . m s

9 1 . 0

5 5 . 0

1 3 3 . 1

1 7 8 . 1

2 1 5 . 1

2 5 2 . 2

2 8 9 . 1

3 2 6 . 2 3 6 0 . 2 4 0 2 . 3 4 4 0 . 3 4 7 6 . 3

Very Dirty Source:

Background

Spectrum

50,000

5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0 5 0 0

0

5 0 0 0

1 0 0 0 0

1 5 0 0 0

2 0 0 0 0

2 5 0 0 0

3 0 0 0 0

3 5 0 0 0

4 0 0 0 0

4 5 0 0 0

5 0 0 0 0

5 5 0 0 0

6 0 0 0 0

6 5 0 0 0

7 0 0 0 0

7 5 0 0 0

m / z - - >

A b u n d a n c e

A v e r a g e o f 1 0 0 . 0 0 9 t o 1 1 0 . 0 2 7 m i n . : E I - b a c k g r d - r e p 3 . D \ d a t a . m s

7 8 . 14 5 . 1 2 0 6 . 9 2 8 1 . 11 3 4 . 9 3 5 5 . 1 4 4 5 . 52 4 1 . 61 6 8 . 1 3 2 0 . 6 3 8 8 . 9 4 7 7 . 9

After Cleaning

with H2

50,000

5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0 5 0 0

0

2 0

4 0

6 0

8 0

1 0 0

1 2 0

1 4 0

1 6 0

1 8 0

2 0 0

2 2 0

2 4 0

m / z - - >

A b u n d a n c e

A v e r a g e o f 1 0 0 . 0 0 9 t o 1 1 0 . 0 2 7 m in . : E I - b a c k g r d - r e p 3 . D \ d a t a . m s

7 8 . 1

4 5 . 1 2 0 6 . 9

2 8 1 . 1

1 3 4 . 9 3 5 5 . 1

4 4 5 . 52 4 1 . 61 6 8 . 1 3 2 0 . 6 3 8 8 . 9 4 7 7 . 9

Expanded scale

50


23 August 2013

Cleaning Restores Analyte (OFN) Detection Comparable to manual cleaning?

4 . 1 0 4 . 1 2 4 . 1 4 4 . 1 6 4 . 1 8 4 . 2 0 4 . 2 2 4 . 2 4 4 . 2 6 4 . 2 8 4 . 3 0 4 . 3 2 4 . 3 4 4 . 3 6 4 . 3 8

1 4 0 0 0 0

1 4 2 0 0 0

1 4 4 0 0 0

1 4 6 0 0 0

1 4 8 0 0 0

1 5 0 0 0 0

1 5 2 0 0 0

1 5 4 0 0 0

1 5 6 0 0 0

1 5 8 0 0 0

1 6 0 0 0 0

1 6 2 0 0 0

1 6 4 0 0 0

1 6 6 0 0 0

1 6 8 0 0 0

1 7 0 0 0 0

1 7 2 0 0 0

1 7 4 0 0 0

1 7 6 0 0 0

1 7 8 0 0 0

T i m e - - >

A b u n d a n c e

I o n 2 4 1 . 0 0 ( 2 4 0 . 7 0 t o 2 4 1 . 7 0 ) : O F N - p r e c o n d - 0 - r e p 0 0 . D \ d a t a . m s

4 . 1 0 4 . 1 2 4 . 1 4 4 . 1 6 4 . 1 8 4 . 2 0 4 . 2 2 4 . 2 4 4 . 2 6 4 . 2 8 4 . 3 0 4 . 3 2 4 . 3 4 4 . 3 6 4 . 3 8

0

5 0 0

1 0 0 0

1 5 0 0

2 0 0 0

2 5 0 0

3 0 0 0

3 5 0 0

4 0 0 0

4 5 0 0

5 0 0 0

5 5 0 0

6 0 0 0

6 5 0 0

7 0 0 0

7 5 0 0

T im e - - >

A b u n d a n c e

T I C : O F N - p o s t c o n d - 1 - p r e t u n e - r e p 0 2 . D \ d a t a . m s

S:N > 50 pk-pk

> 200 rms

S:N ≈ 1 pk-pk

> 2 rms

Very dirty

source before

cleaning

After cleaning

with H2


24 August 2013

PAHs on 2 different 7000B MS/MS systems, MRM

Dibenzo(a,l)pyrene, a late eluter

stock configuration

Optimized PAH

Analyzer


25 August 2013

0.750

0.800

0.850

0.900

0.950

1.000

1.050

1.100

1.150

no

rmalized

resp

on

se

pg inj

30 Mix PAH ISTDs, 9 mm DO With 75 uL/min H2 on SQ

Naphthalene D8

Acenaphthene-d10

Phenanthrene D10

Chrysene-D12

Perylene-d12

Continuous

H2 addition

No H2

addition

GC/MS PAH Analysis PAH ISTDs, Cal Range 0.5-500 pg


26 August 2013

GC/MS/MS PAH Analysis PAH ISTDs, Cal Range 1-1000 pg

Initial

data

CCM

Day 1

CCM

Day 3

CCM

Day 12


27 August 2013

Calibration Issues Dibenzo(a,l)pyrene (1-1000 pg, R2 = 0.9785)

Trying to fit the data

to a straight line


28 August 2013

Calibration in Continuous Clean Mode Dibenzo(a,l)pyrene (1-1000pg, R2=0.99998)


29 August 2013

GC/MS/MS PAH Analysis R2 values for calibration 1-1000 pg, Cont. Cleaning Mode

R2 values for 5977A SIM with Continuous Cleaning are nearly

identical to 7000B, across the same 1-1000 pg calibration range

Continuous Continuous

Initial Data Clean Initial Data Clean

R2 R2 R2 R2

Naphthalene 0.9982 0.9999 2,3-Dimethyl anthracene 0.9648 0.9999

1-Methyl naphthalene 0.9981 1.0000 Fluoranthene 0.9978 0.9999

2-Methyl naphthalene 0.9977 1.0000 9,10 Dimethyl anthracene 0.9726 1.0000

1,2-Dimethyl naphthalene 0.9974 1.0000 Pyrene 0.9846 1.0000

1,6-Dimethyl naphthalene 0.9976 1.0000 1-Methyl pyrene 0.9927 0.9997

Acenaphthylene 0.9975 0.9999 Benz (a) anthracene 0.9976 0.9998

Acenaphthene 0.9983 1.0000 Chrysene 0.9976 0.9999

Fluorene 0.9976 1.0000 6-Methyl chrysene 0.9690 0.9998

Phenanthrene 0.9972 0.9999 Benzo (k) fluoranthene 0.9954 1.0000

Anthracene 0.9959 0.9999 Benzo (a) pyrene 0.9576 1.0000

2-Methyl phenanthrene 0.9846 0.9999 Dibenz (a,h) anthracene 0.9581 0.9999

2-Methyl anthracene 0.9846 0.9999 Indeno (1,2,3-c,d) pyrene 0.9642 0.9999

1-Methyl phenanthrene 0.9969 1.0000 Benzo (ghi) perylene 0.9965 1.0000

3,6-Dimethyl phenanthrene 0.9851 1.0000 Dibenzo (a,l) pyrene 0.9788 1.0000


30 August 2013

The Most Comprehensive Solution for the GC/QQQ Analysis of Pesticides and Environmental Pollutants

March 24, 2014


31




*Spraying DDT in neighborhoods

In the 1940s and 1950s

*Children running through the DDT

spray

*Photos from the 2011 movie

Tree of Life

Pesticide Analysis GC/MS/MS Analyzers

Pesticide & Environmental Pollutant Analyzer 2.0

32 September 2013

MS Analyzer Overview

• MRM database with ~1100 compounds and

~8500 optimized transitions including 710+

pesticides and breakdown products

• DVD that shows you how to build an optimized

MRM acquisition method based on your

compound list

• Retention Time Locked separation for reliable

peak identification and quantification

• Multimode inlet for large volume injection

helps optimize detection limit performance

• Capillary Flow Technology Backflush for

faster cycle time and reduced system

maintenance

• Quick-start guide that allows you to quickly

utilize Agilent’s advanced technologies and get

outstanding analytical results immediately after

installation

Classes of Compounds in the Database

Compound Classification Total Number

Pesticides (fungicides, herbicides, insecticides, rodenticides and others) 675

Breakdown Products 42

Deuterated Compounds 6

Polybrominated Diphenyl Ether (PBDE) 4

Polybrominated Biphenyl (PBB) 1

Polychlorinated Biphenyl (PCB) 209

Polycyclic Aromatic Hydrocarbon (PAH) 26

Phthalates 17

Additional Semi-volatile Pollutants 94


40 Minute Constant

Flow Method

20 Minute Constant

Flow Method

40 Minute Constant

Pressure Method

Column(s) 2 x 15m 2 x 15m 1 x 30m

Backflushing type Mid-point Mid-point Post-column

# Targets ~300+ ~200+ ~300+

Configuration G3445B Opt. 412 G3445B Opt. 412 G3445B Opt. 411

Ease of re-lock

Inlet

MS

Aux EPC

Column

PUU

Post-column backflushing

Restrictor

Inlet

MS

Aux EPC

Column #1 Column #2

PUU

Mid-point backflushing

Pre-Configured Analyzer GC Methods


New Methods Now Available:

5x15 Mid Column Constant Flow Method

15 M Post-Column Constant Pressure Method

Improving speed and sensitivity of the analysis!

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)

Flexibility: multiple transitions; 2 classifications; 3 RTs and RIs

March 24, 2014 35

(Color Scales): Red denotes strong

intensity and blue denotes weak

intensity among ALL transitions.

36

Flexibility: Excel Format, Relative and Absolute Transition Intensity

MassHunter Format

One Quant and several Qualification

ions for each compound

The absolute and relative

intensities of transitions

Compound names in Chinese and Japanese

March 24, 2014

It’s Demo Time!

2013.06.18

https://www.youtube.com/results?search_q

uery=Pesticides+%26+Pollutants+MRM+D

atabase+Overview&sm=12

C:\Users\lfs-

wyliep\Documents\Pesticides\Pesticide

Method Builder based on Kai Database

Feb 2014

MRM Database Videos

MRM Database:

New Interface

Our Analyzers all use Backflushing!

March 24, 2014


38

Matrix Compounds May Be Left in the Column After Each Injection

Column Inlet

After Run 1

After Run 2

After Run 3

Carrier Flow

• These heavy matrix materials build up and travel further into the column with each

injection.

• This build-up of heavy materials can cause retention time shifts, peak distortion,

higher bleed, and loss of sensitivity

1 1 1

1 1 1 2 2 2

1 1 1 2 2 2 3 3 3

Mid-column, post run back flush

Purged Union

MS

Inlet

Inlet EPC

P1

Column #1

Aux

EPC

P2

Split

Vent

Purged Union

During the run, P1 > P2 , Carrier gas flows towards MS

Column #2

Column #1

Purged Union

MS

Inlet EPC

P1

Aux

EPC

P2

Split

Vent


During the run, P1 > P2 , Carrier gas flows towards MS

Analytes of

interest

Matrix components

Pesticides in Tea

7000 GC-QQQ

Using G9250AA Database

DRS- Food Applications

July 4th 2012

Column #2

Column #1

Purged Union

MS

Inlet EPC

P1

Aux

EPC

P2

Split

Vent

Inlet


During post run back flush P1 < P2 , Carrier flow reversed in column

DRS- Food Applications

July 4th 2012

Column #2

What Happens when you Don’t Backflush

March 24, 2014

43

9x10

1

2

3

9x10

1

2

3

9x10

1

2

3

Counts vs. Acquisition Time (min)

4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34

Acetonitrile blank analysis after the dandelion root powder analysis without backflushing

and run time of 20 min

Run time = 20 min

Run time = 35 min (additional 15 min at 290°C)

Matrix peaks observed in two

subsequent blank injections!

At least additional 10 min

at 290°C needed to elute

the less volatile matrix

components (e.g. sterols).

Dandelion root powder full scan (m/z 45-650) analysis without backflushing

Results provided by Dr. Katarina Mastovska, Covance Laboratories

The Purged Ultimate Union (PUU) configurations Aux EPC

Column 1 Column 2

PUU MSD

or

QQQ

or

Q-TOF

inlet MS (Turbo Only)

Vocabulary

Post-column

PUU

restrictor Capillary column

inlet Mid-column PUU

Capillary column Capillary column

MS (Turbo or Diff)

Purged

Ultimate

Union

inlet Mid-column PUU

Longer capillary column Short

capillary column

MS (Turbo or Diff)

March 24, 2014 44

M

45

Backflushing Eliminates Less Volatile Matrix Components (Using Mid-Column Backflush)

Dandelion root powder full scan (m/z 45-650) analysis with backflushing

Results provided by Dr. Katarina Mastovska, Covance Laboratories

9 x10

0.5

1

1.5

2

2.5

3

9 x10

0.5

1

1.5

2

2.5

3


4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34

Acetonitrile blank analysis (no backflushing , additional 15 min at 290 ° C)

after the dandelion root powder analysis with backflushing

No matrix peaks from the previous injection observed!

Run time = 20 min

Backflushing starts

(after deltamethrin safely elutes from the first column)

Last analyte RT = 18.45 min

Deltamethrin ( m/z 253 >172)

2 x10

0

1

2

3

4

5

6


18.2 18.3 18.4 18.5 18.6

9 x10

0.5

1

1.5

2

2.5

3

9 x10

0.5

1

1.5

2

2.5

3


4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34

Acetonitrile blank analysis with extended run

No matrix peaks from the previous injection observed!

Run time = 20 min

Backflushing starts

Last analyte RT = 18.45 min

Deltamethrin ( m/z 253 >172)

March 24, 2014

Summary

Agilent Analyzers:

• Get you up and running before the service engineer leaves your

lab!

• Save you from method development

• Can expand your scope of analytes

• Are pre-configured and pre-tested in Agilent factory

• Are based on what we know works

• Use backflushing to reduce/eliminate source cleaning, carryover,

column clipping, interferences, etc.

Yes, they cost a little more, but they save you time and $ in the end!

March 24, 2014


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