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)
1.6
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5 76 8 109 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35
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
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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
ed a
voca
do
120
100
80
60
40
20
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
fied
in b
ovin
e liv
er sa
mple
s
30
25
20
15
10
5
0
EMR—Lipid cleanup
REC<70% REC in 70–120%REC>120
C18/PSA cleanup Zirconia sorbent cleanup
EMR—LIPID
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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
3.2
3
2.8
2.6
2.4
2.2
2
1.8
1.6
1.4
1.2
1
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0.6
0.4
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0
+MRM (324.1 -> 296.1)AVBVR POQ4.d
x103
1.0
0.5
0
Acqusition Time (min) 14.2 14.46 15 15.4 15.6
Coun
ts
14.863 min.
x104
2.6
2
1.6
0.8
0.5
0.2
-0.2
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
3.25
2.25
1.25
0.75
-0.25
Acqusition time (min) 20.4 20.6 20.8 21 21.2
20.788 min.
+MRM (183.1 -> 168.1)AV MBPI-a-CD C2 spike 50 ppb-1.D
3.2
3
2.8
2.6
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2
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1.4
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1
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0
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) AVZ-Sep+ POQ 4.d
14.863 min.
+MRM (151.0 -> 79.1)AV Z-Sep+ C5 spike 50 ppb-1.d x105
1.6
1.2
1.0
0.8
0.5
0.2
-0.1
Acqusition time (min) 12.7 12.9 13.2 13.4 13.6
Coun
ts
13.163 min.
x104
7
6
5
4
2
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
1.4
1.2
1.0
0.8
0.5
0.2
-0.1
Acqusition time (min) 12.7 12.9 13.2 13.4 13.6
Coun
ts
*13.174 min.
x104
7
6
5
4
2
1
0
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
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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
are
a
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0
0
EMR—Lipid cleanup. Response drops – 4%C18/PSA cleanup. Response increases – 35%Zirconia sorbent cleanup. Response drops – 50%
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Injections of avocado extract samples on GC/QQQ
Relat
ive a
bund
ance
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unin
g io
n (%
)
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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
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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
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© Agilent Technologies, Inc. 2016 Printed in the USA March 18, 2016 5991-6052EN