Agilent Enhanced Matrix Removal—Lipid

LOSE THE LIPIDS, FIND YOUR ANALYTES

Figure 1. GC/MS full-scan chromatogram overlay of an untreated QuEChERS avocado extract (black), compared to traditional C18/PSA cleanup (red) and an extract treated with Agilent Enhanced Matrix Removal—Lipid (blue).

Counts vs. acquisition time (min)

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Avocado — Quechers extract before dSPE Avocado — Quechers extract with C18/PSA cleanup Avocado — Quechers with EMR—Lipid cleanup

92% Matrix Removal with EMR—Lipid

ARE LIPIDS WEIGHING YOUR SAMPLES DOWN?

Interference from lipids is a problem for labs measuring trace residues in fatty foods or complex biological matrixes. Lipids can build up in the instrument and column, decreasing lifetime and reducing analyte sensitivity due to ion suppression. The need for MS maintenance increases too, because of lipid deposits on the source. The need for lipid removal is well understood, but current methods often sacrifice analyte recovery, removing some of your target analytes along with the lipids.

Now, you don’t have to choose between lipid removal and analyte recovery, because innovative Agilent Enhanced Matrix Removal—Lipid delivers the most complete matrix removal and analyte recovery of any sample prep product.

Enhanced Matrix Removal—Lipid, UNLIKE any other type of sample prep, is a unique sorbent that selectively removes lipids in complex matrixes and challenging high-fat samples such as avocado, so you can remove lipids without losing your analytes.

AGILENT ENHANCED MATRIX REMOVAL—LIPID

2

STANDARD QuEChERSExtraction/partition (6 steps)

Mix and centrifuge

Transfer to dSPE (sorbents)

Mix and centrifuge

Evaporate/reconstitute or dilute

Filter out precipitate

Transfer to A/S vial

The innovative sorbent in EMR—Lipid replaces C18/PSA in your QuEChERS methodology to significantly reduce matrix effects and improve analyte recoveries. It can be universally applied to the analysis of polar, mid-polar and non-polar target analytes, providing effective matrix removal.

*Note: Polish step is omitted for tetracycline analysis.

EMR—LIPID QuEChERSExtraction/partition (6 steps)

Mix and centrifuge

Transfer to dSPE (EMR—Lipid & H2O)

Mix and centrifuge

Polish and dry*

Evaporate/reconstitute or dilute

Transfer to A/S vial

Sample Type Removal (%)

Avocado 92

Olive oil 73

Avocado oil 82

Canola oil 75

Beef liver 97

Wet cat food 91

Paprika 91

Cumin 72

Hops 57

Tumeric 47

Black pepper 22

Onion 41

Strawberry 10

Plum 12

Red pepper 61

Spinach 61

Orange 52Apple 66

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MINIMIZE LIPIDS. MAXIMIZE RESULTS.

Analy

te re

cove

ry %

(n=6

) in

50 p

pb p

estic

ides f

ortifi

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voca

do

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0Methamidophos

EMR—Lipid cleanupC18/PSA dSPE cleanupZirconia sorbent cleanup

Thiophanate methtyl

2,4-D AcidBentazone TPPDichlorprop Penconazole EPN Captafol

EMR—Lipid significantly removes matrix contributions, improving recovery across many analytes and minimizing your need for separate workup and methods.

Higher efficiency matrix removal with EMR—Lipid produces higher precision and greater accuracy in results.

Figure 2. Recovery data for multiple pesticide residue analysis in avocado, showing some of the 73 pesticides analyzed. Using Agilent Enhanced Matrix Removal—Lipid, 92% of the pesticides fell within the acceptable recovery range of 70 to 120%.

Figure 3. Number of analytes with % recoveries within the acceptable % recovery range of 70-120% for the analysis of vet drugs in Bovine Liver, demonstrating the higher number of acceptable results after Agilent Enhanced Matrix Removal—Lipid cleanup vs zirconia sorbent cleanup. An

alyte

s Rec

over

y % (n

=6) i

n 50

ppb

vet d

rugs

forti

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in b

ovin

e liv

er sa

mple

s

30

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EMR—Lipid cleanup

REC<70% REC in 70–120%REC>120

C18/PSA cleanup Zirconia sorbent cleanup

EMR—LIPID

4

Chromatographic benefits of sample preparation using EMR—Lipid

Efficiently removing lipids from samples without removing analytes is the key to improving chromatographic performance for the best quality data, especially with high-sensitivity MS detectors.

An EMR—Lipid QuEChERS protocol considerably improves accuracy, reproducibility, and low-level quantitation when using GC/MS and LC/MS (Figure 4).

Figure 4. Improvements in chromatography can be seen in the analysis of samples prepared with Agilent Enhanced Matrix Removal—Lipid, including better sensitivity due to reduced matrix ion suppression, better signal-to-noise ratio, and fewer interferences providing accurate integration with GC or LC triple quadrupole systems.

BENEFIT BETTER ANALYTE SENSITIVITY

IMPROVED S/N RATIO LESS INTERFERENCES FOR ACCURATE INTEGRATION

Example EPN in avocado on LC-QQQ

Captan in avocado on GC-QQQ

Permethrin in avocado on GC-QQQ

EMR—Lipid cleanup

Zirconia sorbent cleanup

C18/PSA cleanup

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+MRM (324.1 -> 296.1)AVBVR POQ4.d

x103

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Acqusition Time (min) 14.2 14.46 15 15.4 15.6

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14.863 min.

x104

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Acqusition time (min) 12.7 13 13.2 13.4 13.6

13.163 min.

+MRM (151.0 -> 79.1)AV MBPI-a-CD C2 spike 50 ppb-1.D x104

5

4.25

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-0.25

Acqusition time (min) 20.4 20.6 20.8 21 21.2

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+MRM (183.1 -> 168.1)AV MBPI-a-CD C2 spike 50 ppb-1.D

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Acqusition time (min) 14.2 14.46 15 15.4 15.6

Coun

ts

+MRM (324.1 -> 296.1) AVZ-Sep+ POQ 4.d

14.863 min.

+MRM (151.0 -> 79.1)AV Z-Sep+ C5 spike 50 ppb-1.d x105

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Acqusition time (min) 12.7 12.9 13.2 13.4 13.6

Coun

ts

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x104

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1

0

Acqusition time (min) 20.4 20.6 20.8 21 21.2

20.819 min.

+MRM (183.1 -> 168.1) AV MZ-Sep+ C5 spike 50 ppb-1.D

x103

1.0

0.5

0

Acqusition time (min) 14.2 14.46 15 15.4 15.6

Coun

ts

+MRM (324.1 -> 296.1)AVC8 PR-Q3.d

14.855 min.

+MRM (151.0 -> 79.1)Post-S 50 ppb Fatty cSPE C1-2.D x105

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Acqusition time (min) 12.7 12.9 13.2 13.4 13.6

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*13.174 min.

x104

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Acqusition time (min) 20.4 20.6 20.8 21 21.2

20.833 min.

+MRM (183.1 -> 168.1) AV Fatty dSPE spike 50 ppb-1R.D

5

Without effective sample cleanup, analytical efficiency and quality are quickly compromised as fatty matrixes build up in the instrument and column. With EMR—Lipid, system performance is maintained even after 100 injections of a fatty-matrix sample like avocado. Reduced maintenance allows for increased sample throughput and enables you to use your assets to their fullest extent, maximizing productivity in your lab.

Faster sample prep streamlines lab productivity

Figure 5. Analyte response across 100 avocado sample injections. Triphenyl phosphate (TPP) is a commonly used internal standard. Signal suppression or enhancement can result from insufficient cleanup of samples, which can contribute to poor data quality, errors, and re-running samples. The superior matrix removal ability of Agilent Enhanced Matrix Removal—Lipid, results in a cleaner source and more consistent MS response over time, for higher quality data, fewer re-runs, and reduced need for time-consuming troubleshooting and source maintenance.

Figure 6. GC/MS source conditions during 2500 injections of avocado samples, demonstrating significantly reduced frequency of MS source maintenance (cleaning or replacement) when using Agilent Enhanced Matrix Removal—Lipid.

With EMR—Lipid there is less need for system maintenance and calibration due to fewer sample matrix interferences. As a result, fewer samples need to be re-run. This advantage lets you operate at higher throughput, resulting in cost savings and a more efficient lab.

TPP

peak

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a

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EMR—Lipid cleanup. Response drops – 4%C18/PSA cleanup. Response increases – 35%Zirconia sorbent cleanup. Response drops – 50%

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Injections of avocado extract samples on GC/QQQ

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Injections of avocado samples after EMR—Lipid cleanup

EM V

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METHOD PERFORMANCE CRITERIA >1600V needs EM replacement Min 70 Min 5

EM voltageRel. abundance MS ion 219Rel. abundance MS ion 502

PARAMETER

6

Faster sample prep streamlines lab productivity Over a hundred runs of fatty sample analysis, the consistently better, effective cleanup of EMR—Lipid results in lower % RSDs and greater confidence in results, compared to alternative QuEChERS procedures. Higher quality data with better precision results in less need for data re-verification, justification and fewer costly re-runs.

Figure 7. Reproducibility of pesticides analyzed (%RSD) over multiple injections of avocado samples on GC/QQQ. 50 ppb fortified avocado samples were tested every five injections, and avocado matrix blanks were injected in between. RSD > 20% are considered as unacceptable and marked in red.

PesticidesAnalytes RSD over 100 injections on GC/QQQ (n = 20)EMR—Lipid

CleanupC18/PSA Cleanup

Zirconia sorbent Cleanup

Dichlorvos 6.2 10.5 16.8

2-Phenylphenol 7.0 13.6 19.5

Ethalfluralin 12.4 18.8 32.0

Sulfotep 7.1 11.8 17.2

Atrazine 6.8 12.2 19.1

Lindane 8.5 10.8 20.0

Chlorothalonil 12.5 11.7 37.4

Diazinon 6.6 11.7 16.9

Chlorpyriphosmethyl 8.4 8.9 14.9

Dichlofluanid 11.7 9.0 25.9

Aldrin 9.8 19.3 25.7

Tolylfluanid 10.5 6.6 17.8

Captan 29.9 51.9 47.1

Procymidone 6.8 14.3 22.5

Bupirimate 6.8 10.4 20.7

Endrin 8.3 12.6 24.1

Endosulfan sulfate 8.5 12.1 22.4

DDT 21.6 22.4 42.6

Iprodione 11.0 10.7 40.0

Permethrin 6.8 11.8 18.8

Parathion ethyl 11.8 7.2 13.0

TPP 9.1 19.9 28.3

The benefits of using new and innovative EMR—Lipid are clear Improved productivity: better sensitivity and signal-to-noise from fewer matrix interferences enable faster data processing, and greater sample throughput.

Reduced lab costs: cleaner samples using EMR—Lipid can significantly reduce the need for MS source maintenance, giving you more time to analyze samples while spending less time on costly troubleshooting, downtime, and instrument repair.

Part Number Description 5982-1010 Bond Elut EMR—Lipid dSPE 5982-0101 Bond Elut EMR—Lipid Final Polish Tube 5982-0102 Bond Elut EMR—Lipid MgSO4 Polish Pouch

Simplified workflows: standardize on an easy-to-use single-sorbent procedure that maximizes analyte recovery from a wide variety of fatty samples. Save time and money by reducing material costs, inventory, training time, and documentation, thereby streamlining your lab productivity.

Higher quality results: a cleaner sample profile leads to greater data integrity and confidence in results, faster data processing, and fewer re-runs.

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The best analysis requires the best overall workflowExplore more food testing solutions at www.agilent.com/chem/food

Increase analysis throughput with current instruments and minimal investment—check how to increase your laboratory productivity here:

Liquid chromatography analysis workflow www.agilent.com/chem/ProductivityLC

Gas chromatography analysis workflow www.agilent.com/chem/ProductivityGC

Learn morewww.agilent.com/chem/emr-lipid

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© Agilent Technologies, Inc. 2016 Printed in the USA March 18, 2016 5991-6052EN