lose the lipids, find your analytes

Agilent Enhanced Matrix Removal—Lipid
LOSE THE LIPIDS,
FIND YOUR ANALYTES
AGILENT ENHANCED MATRIX REMOVAL—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.
Avocado — Quechers extract before dSPE
Avocado — Quechers extract with C18/PSA cleanup
Avocado — Quechers with EMR—Lipid cleanup
x106
1.6
92% Matrix Removal with EMR—Lipid
1.5
1.4
1.3
1.2
1.1
1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
Counts vs. acquisition time (min)
23
24
25
26
27
28
29
30
31
32
33
34
35
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).
2
STANDARD QuEChERS
EMR—LIPID QuEChERS
Extraction/partition (6 steps)
Extraction/partition (6 steps)
Mix and centrifuge
Mix and centrifuge
Transfer to dSPE (sorbents)
Transfer to dSPE (EMR—Lipid & H2O)
Mix and centrifuge
Mix and centrifuge
Evaporate/reconstitute or dilute
Polish and dry*
Filter out precipitate
Evaporate/reconstitute or dilute
Transfer to A/S vial
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.
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
52
Apple
66
3
EMR—LIPID
MINIMIZE LIPIDS.
MAXIMIZE RESULTS.
Analyte recovery % (n=6) in 50 ppb pesticides fortified avocado
120
EMR—Lipid significantly removes matrix
contributions, improving recovery across
many analytes and minimizing your need
for separate workup and methods.
EMR—Lipid cleanup
C18/PSA dSPE cleanup
Zirconia sorbent cleanup
100
80
60
40
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%.
20
0
Analytes Recovery % (n=6) in 50 ppb vet drugs fortified in bovine liver samples
Methamidophos Thiophanate Bentazone
methtyl
Dichlorprop Penconazole
TPP
EPN
Captafol
REC<70%
REC in 70–120%
REC>120
30
Higher efficiency matrix removal with
EMR—Lipid produces higher precision
and greater accuracy in results.
25
20
15
10
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.
5
0
EMR—Lipid cleanup
4
2,4-D Acid
C18/PSA cleanup
Zirconia sorbent cleanup
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).
BENEFIT
Example
BETTER ANALYTE
SENSITIVITY
3.2
EPN
in avocado on LC-QQQ
3
IMPROVED S/N RATIO
LESS INTERFERENCES FOR
ACCURATE INTEGRATION
Captan in avocado on GC-QQQ
Permethrin in avocado on GC-QQQ
2.8
2.6
+MRM (324.1 -> 296.1)
AVBVR POQ4.d
2.4
103
x
2.2
2.6
Counts
1.0
1.8
1.6
1.2
0
1
14.2 14.46
3.2
0.8
5
15
15.4
2.25
1.25
0.2
0.75
-0.2
-0.25
12.7
2.6
105
+MRM (324.1 -> 296.1)
AVZ-Sep+ POQ 4.d
2.4
0
x
Counts
1.8
1.6
1.4
1.2
Counts
x
2
1.0
0.5
14.863 min.
1
15
15.4
6
5
0.8
4
105
x
Counts
Counts
0.5
14.855 min.
13.2
13.4
15
15.4
15.6
Acqusition time (min)
20.8
21
21.2
Acqusition time (min)
104
7
x
1.2
6
1.0
5
0.8
4
+MRM (183.1 -> 168.1) AV
Fatty dSPE spike 50 ppb-1R.D
20.833 min.
2
0.5
*13.174 min.
1
0
-0.1
14.2 14.46
20.4 20.6
13.6
+MRM (151.0 -> 79.1)
Post-S 50 ppb Fatty cSPE C1-2.D
0.2
0
+MRM (183.1 -> 168.1) AV
MZ-Sep+ C5 spike 50 ppb-1.D
20.819 min.
0
12.9
1.4
1.0
21.2
1
Acqusition time (min)
103
x
0
21
2
13.163 min.
12.7
15.6
+MRM (324.1 -> 296.1)
AVC8 PR-Q3.d
0.2
104
7
x
1.0
0.5
20.8
Acqusition time (min)
1.2
Acqusition time (min)
0.4
20.4 20.6
13.6
-0.1
14.2 14.46
0.6
13.4
+MRM (151.0 -> 79.1)
AV Z-Sep+ C5 spike 50 ppb-1.d
0.2
0
0.8
13.2
1.6
103
2.2
13
Acqusition time (min)
2.8
0.4
0.2
3.25
0.5
15.6
+MRM (183.1 -> 168.1)AV
MBPI-a-CD C2 spike 50 ppb-1.D
20.788 min.
4.25
0.8
Acqusition Time (min)
0.63
C18/PSA cleanup
104
x
13.163 min.
1.6
0.5
1.4
Zirconia sorbent cleanup
+MRM (151.0 -> 79.1)AV
MBPI-a-CD C2 spike 50 ppb-1.D
2
2
EMR—Lipid cleanup
104
x
14.863 min.
12.7
12.9
13.2
13.4
13.6
Acqusition time (min)
20.4 20.6
20.8
21
21.2
Acqusition time (min)
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.
5
Faster sample prep streamlines lab productivity
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.
20000
18000
16000
14000
TPP peak area
12000
10000
8000
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.
6000
4000
EMR—Lipid cleanup. Response drops – 4%
C18/PSA cleanup. Response increases – 35%
Zirconia sorbent cleanup. Response drops – 50%
2000
0
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
130
1600
120
0
1400
110
1200
90
80
1000
70
800
60
50
PARAMETER
METHOD PERFORMANCE CRITERIA
EM voltage
Rel. abundance MS ion 219
Rel. abundance MS ion 502
40
30
>1600V needs EM replacement
Min 70
Min 5
600
400
20
200
10
0
0
0
500
1000
1500
Injections of avocado samples after EMR—Lipid cleanup
6
EM Voltage
Relative abundance for tuning ion (%)
100
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.
2000
2500
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.
Pesticides
Analytes RSD over 100 injections on GC/QQQ (n = 20)
EMR—Lipid
Cleanup
C18/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
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.
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.
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.
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
7
The best analysis requires the best overall workflow
Explore 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 more
www.agilent.com/chem/emr-lipid
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© Agilent Technologies, Inc. 2016
Printed in the USA March 18, 2016
5991-6052EN