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 Buy online www.agilent.com/chem/store Find a local Agilent customer center in your country www.agilent.com/chem/contactus USA and Canada 1-800-227-9770 [email protected] Europe [email protected] Asia Pacific [email protected] This information is subject to change without notice. © Agilent Technologies, Inc. 2016 Printed in the USA March 18, 2016 5991-6052EN
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