FOOD TESTING APPLICATIONS - LECO Corporation

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FOOD TESTING APPLICATIONSeBook LECO Corporation –company facts GC- and GC GC-TOFMSinstrumentation Specific LECO GC-TOFMSinstrument features Separation Scienceproduct portfolio Selection of LECO SepSciApp Notes LECO Food TestingBibliographyNext Page

LECO CORPORATIONSOME COMPANY FACTS

SOME COMPANY FACTSLECO CORPORATIONEstablished in 1936 by Carl Schultz,the Laboratory Equipment Companyintroduced what would be the firstrapid carbon determinator to theAmerican iron and steel industry.Today, over 80 years later, LECOcontinues to be a family-ownedcompany in its third generation ofleadership and is recognised globallyas a leader in the developmentof high-quality elemental andthermal analysis equipment, massspectrometers and chromatographs,metallography and opticalequipment, and consumables.Our headquarters in St. Joseph,Michigan, USA, is comprised ofseveral facilities each dedicatedto improving customer success,including state-of-the-art researchand development centers and ruggedmanufacturing facilities. Through thisvertical integration system, we areable to maintain strict control over themanufacturing and assembly processin accordance with our qualitystandards.LECO established its first internationaloffice in Germany in 1967, andsince that time has grown to includeover 25 worldwide subsidiaries anddistributors who are authorised to sellour equipment to over 75 countriesaround the Globe.3 // LECO Food 2020

LECO’S KEY MARKETSEnergy & FuelsWhile LECO has continued to be a leader in carbon/sulfur testing of coal andcoke, it has since expanded into biofuels, biomass, oil additives, petroleumproducts. Ensuring existing sources, and analysing fuels of the future –LECO technology is here to validate their potential and quality.Environment & AgricultureLECO instruments helps to monitor environmental impact, manage agricultural resourcesmore efficiently by monitoring composition of arable soils, crop and fertilisers;determining optimum nutrition values for animal feed.Food SafetyMulti residue methods and screening all at once; food contamination;authenticity or traceability: LECO provides solutions with unrivalledperformance, sensitivity, speed and robustness.Life Science & PharmaceuticalAcademic research and drug discovery requires the instrumentation that goes beyondnormal expectations. Empowered by advanced LECO mass spectrometry be moreconfident in your assignments.MetabolomicsAs the established leader in GCMS metabolomics, LECO products deliver theaccuracy, resolving power, deconvolution, and speed to characterise the mostcomplex biological systems. Our instrumentation has been validated by theindustry's most demanding researchers.Metallurgy & MetalsWith a global reputation for rapid, accurate analysis in iron, steel, alloys, refractorymetals, and ores, LECO instruments have become the brand leader for these markets.4 // LECO Food 2020

GC- AND GC GC-TOFMSINSTRUMENTATION

BENEFITSOF GC GCComprehensive two-dimensionalgas chromatography (GC GC) is ananalytical technique that has beenaround for over 25 years.GC GC increases separation capacity by using twoseparate columns with orthogonal selectivity connectedin series through a modulator (Figure 1). The modulatorrapidly traps and "injects" the effluent from the firstdimension column onto the second dimension.Figure 1: Principle of GC GCThe result of a GC GC analysis is a chromatographicplane (contour plot) (Figure 2), that depicts theseparation over the nonpolar and polar columns.The chromatographic separation space is dramaticallyincreased compared to a conventional 1D-GC.Other benefits of GC GC are structured twodimensional chromatograms (i.e. contour plots),and sensitivity enhancement. Research has shownthe advantages of GC GC in a wide variety ofapplications (e.g. environmental, metabolomics,petroleum, food safety, fragrance).The merits of GC GC as a separation science are clear,but how will it benefit a routine laboratory?View the full article “Benefits of Comprehensive GasChromatography (GC GC) for Routine Laboratory”Figure 2: Data Conversion for Visualisation6 // LECO Food 2020

BENEFITSOF TIME-OF-FLIGHT MASS SPECTROMETRYA time-of-flight mass spectrometer (TOFMS) for gaschromatography (GC) (Figure 3) is the right choice forcomplex samples, targeted and non-targeted analysis andfast GC or GC GC.Time-of-flight mass spectrometry (TOF-MS) is probably thesimplest method of mass measurement to conceptualise.The ion’s mass-to-charge ratio is determined via a timemeasurement (Figure).The ability to collect a full mass range without sacrificingdata acquisition speed or sensitivity is perfectly suited fornon-targeted analyses. Using a non-targeted approachis beneficial for discovery-type work. A TOFMS spectrumhas better spectral continuity across a peak than with ascanning mass analyser (Figure 4). Spectral continuityis important for maximising the performance of massspectral deconvolution algorithms, which results also inhigher library matches.Figure 3: GC-TOFMS SetupTOFMSGC PeakScanning MSA targeted analytical method also benefitsfrom acquiring a full mass range. Dataprocessing methods including the TargetAnalyte Finding feature can be used forboth qualitative analysis of sample dataand quantitation. View the full article “Benefits of Equipping yourLab with a Time-of-Flight Mass Spectrometer”Figure 4: Spectral Continuity7 // LECO Food 2020

SPECIFIC LECO GC-TOFMSINSTRUMENT FEATURES

STAY CLEAN ION SOURCE STABILITYFouled ion sources and related issues are often timeconsuming to diagnosis and resolve. A definitivediagnosis can only be achieved after other preventativemaintenance steps (inlet maintenance, column trimming,etc.) have been tried and tested. Once the source hasbeen pinpointed as the issue, users have to clean thesource before proceeding.Even routine, scheduled preventative cleaning leadsto system downtime In less controlled environments theincremental contamination of an ion source may not benoticed until long past the point of compromised results orimpacting the stability of the overall system.Worse still, tuning routines will typically compensatefor the loss in signal by increasing various voltages,not the least of which is at the detector. This decreasesthe detector‘s operational life, requiring additionalmaintenance time to resolve.Figure 5: LECO StayClean ion sourceFor these reasons, LECO has specifically designed thePEGASUS BT systems with an ion source (Figure 5) thatvirtually eliminates the need for removal and cleaning.View the application note, which provides significant evidencethat the LECO StayClean ion source actually stays clean.9 // LECO Food 2020

LECO MULTI-MODE SOURCE IONIZATION SOURCE FOR GASCHROMATOGRAPHY MASS SPECTROMETRYThe innovative Multi-Mode Source (MMS ) takes allof the advantages of the three most common ionizationmodes – Electron Ionization (EI), Positive ChemicalIonization (PCI), and Negative Chemical Ionization(NCI/ECNI) – and combines them into one easy-to-usesource. No more hardware switching, no more alignmentissues: with the MMS, changing ionization modes is aseasy as a click of a button.The new MMS has great mass accuracy and highresolution on pseudo-molecular ions, which complementsthe traditional Electron Ionization Source (HR-EI) toprovide the comprehensive characterization of unknowns.By not touching the hardware, peaks stay alignedbetween the ionization modes. Each of the three modes isavaible for GC-MS and GC GC-MS analyses on both thePEGASUS GC-HRT and the Pegasus GC-HRT 4D.Don’t limit yourself to just one approach. Ask about thenew MMS to see what you’ve been missing!10 // LECO Food 2020

LECO MODULATORPORTFOLIOGC GC offers dramatic improvements over traditionalGC for the analysis of complex mixtures. This is due tosignificantly increased chromatographic resolution. Themodulator, considered the heart of the GC GC system,is a device which injects the effluent from the primarycolumn to the secondary column. There are two primaryforms of modulators in GC GC; thermal- and flow-based.These techniques are described in general terms, but withfocus on flow modulation.Thermal-based modulators (Figure 6) rely on a coolingmechanism to trap eluent from the first column, followedby heating to inject the eluent onto the second columnfor further separation. These modulators use of acryogen such as liquid nitrogen for optimal cold-trappingperformance.Stage 2Cold JetStage 2Hot JetStage 1Cold JetStage 1Hot JetFigure 6: Thermal ModulatorFlow-based modulation (Figure 7) relies on eitherswitching valves to inject on-column, or in some cases,combining valves with highly different flows to flush asample loop onto the second column. Both types providea GC GC alternative that is virtually consumablefree. The choice of which GC GC approach is mostappropriate depends on the application that will beperformed on a particular system. View the full article FLUX GC GC: The operation, use,and concepts behind a diverting flow techniqueFigure 7: Flow Modulator11 // LECO Food 2020

LECO ChromaTOF SOFTWARELECO‘s ChromaTOF software is uniquely designed toprocess and analyse the large amounts of data that areacquired with our time-of-flight instruments.ChromaTOF offers seamless control of both the instrumentand its accessories, as well as an intuitive interface withhighly integrated data processing.ChromaTOF is the first mass spectrometrydata system to fully accommodatemultidimensional chromatographicdata (GC GC).Benefits of LECO ChromaTOF Single software platform Automatic tuning within user-definedQuality Control methods Intuitive Acquisition Method Setup Automated Peak Find using Non-TargetDeconvolution and Library Search Target Analyte Finding and Quantification Semi-Quantitative Analysis for the reportingof non-calibrated compounds Reference Compare tools for sample comparison GC GC enhanced graphics and optimisationtools (Classifications, Filters) Automatically export data to PDF, CSV,ANDI MS, NETCDF, or Raw file formats12 // LECO Food 2020

LECO ChromaTOF TILEANALYTICAL SOFTWAREThe volume of GC GC data can quickly becomeoverwhelming. Multiple tables of thousands of analytescan require months of data mining at a pixel level tofind the minute differences between data sets, and eventhose results are plagued with false positives from normalchromatographic variation.ChromaTOF Tile is an enablingtechnology that has reduced our peakpicking time from 10 days to 10 minutes.We are now comparing groups ofpeak-rich samples from complex studiesthat would have previously requiredcomplicated, custom-built solutions.Benefits of LECO ChromaTOF Tile ChromaTOF Tile is a separate, stand-alone productto be used in conjunction with ChromaTOF brandsoftware All of the tables and plots throughout the interface areexportable for more efficient reporting and to allowyou to do more with your data Clean library-searchable spectra is generated fromthe tiling process Areas of the tiles are used to approximately quantifytrends across the samples13 // LECO Food 2020

SEPARATION SCIENCEPRODUCT PORTFOLIO

SEPARATION SCIENCEPRODUCTSPEGASUS BT GC-TOFMSPEGASUS BT 4D GC GC-TOFMSQuadJet SD Industry-leading sensitivityhelps you find and quantify anunlimited number of analytes,while proprietary deconvolutionalgorithms yield clean, highquality spectra E nhanced sensitivity by couplingour benchtop Pegasus BT with ourhigh performance GC GC thermalmodulation system Enhanced separating powerfor complex sample analysis A complete historical record of allcomponents for each sample isretained for future data mining T he tried-and-tested reliability anddurability of our Pegasus brand ina convenient benchtop unit A bility to interrogate challengingsamples where the best sensitivityis needed U nique and powerful ChromaTOF brand software simplifiesquantitation and analyteidentification with features suchas Non Target Deconvolution (NTD ), Target Analyte Find,library searches, and more Easy-to-use ChromaTOF -basedsoftware provides acquisitionprocessing and reportingfunctionality within a singlepackage Classification software featuresimplifies component identification Available Cryogen-free modulatoreliminates the need for LN2dewars StayClean ion source eliminatesthe need for source cleaningView Product Overview15 // LECO Food 2020

SEPARATION SCIENCEPRODUCTSPEGASUS GC-HRT GC-TOFMSPEGASUS GC-HRT 4D GC GC-TOFMS T he highest performance TOF mass spectrometerfor the GCMS market C ombining the highest performance GC GC and TOFon the market gives users an unprecedented ability tointerrogate complex sample F olded Flight Path (FFP ) technology allows users toachieve resolutions of up to 50,000 Employs ChromaTOF software with automatedHigh Resolution Deconvolution (HRD ) and formulageneration for seamless identification of unknowns,plus compatibility with standard GCMS libraries F ind more analytes than ever before and identifycomponents with the ultimate confidence W ith mass accuracies of 1 ppm and peak capacitiesat least two times greater than anywhere else in themarketplace S pectral Analysis Toolkit harnesses the power of MassDefect, Van Krevlen, and RDBE plots to take yourunknown analysis to a new level T he industry‘s most established GC GC systems;thermal modulation with liquid nitrogen or cryogenfree versions 1 ppm mass accuracy identifies unique molecularformula C hemical Ionisation source (HR-CI) provides thesame mass accuracy and high resolution on pseudomolecular ions which complements the traditionalElectron Ionisation source (HR-EI) to providecomprehensive characterisation of unknowns E ncoded Frequent Pushing (EFP ) contributes toincreased sensitivity, expanded dynamic range,and much more I ntegrated software platform acquires data, controls allhardware, and analyses and reports results with ahigh level of automation; tailored to get the most outof HR dataView Product Overview16 // LECO Food 2020

FOOD TESTINGAPPLICATION COMPENDIUM Pesticides in Tomato Yeast Metabolite Characterisation Terpene Profiles in Cannabis Differential Analysis of olive oils Sensory of IPA Beer Pesticides in Tabocco Volatiles in celery PCBS in fish oil supplement Fats in Food Products Determing MOSH/MOAH Pesticide Residue in Strawberries Non-target Detection of Pesticides Roast Level Differentiation of coffee Differentiation of honey aroma

DETERMINATION OF PESTICIDES INTOMATO BY GC GC-TOFMSWITH PEGASUS BT 4DThe tomato is one of the most consumedcrops, globally. It s annual production iscurrently around 130 million tons. The top5 largest tomato producing countries are:China, EU, India, USA, and Turkey. Theyaccount for 70 % of global production.Most freshly harvested tomatoes areimmediately processed into products suchas juice, puree and paste, ketchup/sauceor canned whole. The presence of pesticideresidues in such products can cause a numberof adverse health effects. Therefore, theidentification and quantitation of pesticides intomatoes is an important task for food controlauthorities. A GC GC-TOFMS workflow,including a traditional QuEChERS extractionstep, was developed for the detection andquantitation of targeted pesticides in peeledtomatoes. GC GC technology significantlyincreases the separation efficiency, andultimately allows a better separation of thetarget and non-target analytes from thematrix interferences. This, in combinationwith LECO's Pegasus BT 4D sensitivity, fastacquisition and deconvolution benefits,allowed the measurement of all the pesticidesinvestigated, at required limits of detections tobe performed easily and accurately.Key Words# Pesticides# Food# GC GC# TOFMS# Qualitative andQuantitativeAnalysisView Application NoteAn example of the enhanced resolving power of the GC GC technology, which highlights the chromatographic separation on the "y" axis of thecontour plot.Instrument: LECO PEGASUS BT 4D18 // LECO Food 2020

DETERMINING TERPENE PROFILES OFCANNABIS STRAINS USINGGC AND GC GC WITH HIGHPERFORMANCE TOFMSCannabis is a complex mixture of compounds( 500) including cannabinoids, terpenes,terpenoids, non-cannabinoid phenols,nitrogenous compounds, flavonoids, andcontaminants such as residual solvents andpesticides. It is the total composition ofcannabis that is important in determining itspotency and medicinal effectiveness. This“entourage effect” is a synergistic relationshipthat exists between terpenes, cannabinoids,and potentially other cannabis components.Identification of cannabis components iscritical for the “chemical categorization”of different cannabis strains. GC-TOFMSand GC GC-TOFMS were used to analyzeterpenes from different strains of cannabisGC GC-TOFMS analysis resulted in a 4xincrease in peaks detected and 50 %increase in terpenes identified over thosefound with single dimension GC-MS. Thisadditional information was a direct resultof coupling enhanced multi-dimensionalchromatography with high performanceTOFMS. Robust characterisation wasachieved through spectral similarity searchesof large, well-established databases, withthe enhanced GC GC separation and highquality deconvoluted mass spectral datatherefore providing increased confidence inthese determinations.Key Words# GC GC# PEGASUS BT 4D# Cannabis# GC-TOFMS# High MatrixView Application NoteA) GC-TOFMS TIC for indica terpenes; B) Extracted ion expansion showing coelution in 1D GC-MS; C) Spectrum derived from 1D GC-MS coelution;D) GCxGC-TOFMS contour plot; E) Expansion showing GC GC separated sesquiterpenes dendrasaline and β-calacorene which coeluted in 1DGC-TOFMS; F,G) Clean spectra for chromatographically separated β-calacorene and dendrasalineInstrument: LECO PEGASUS BT 4D19 // LECO Food 2020

CORRELATION OF CHEMICAL ANDSENSORY DATA TO TRACK AGINGOF AN AMERICAN IPA BEERAT DIFFERENT STORAGETEMPERATUREShelf stability and how products change withage and storage condition is an importanttopic to both manufacturers and consumers.Understanding changes in the aroma profileover time can help to understand the shelf lifeof that product and possibly how it can beextended.Gas chromatography coupled to time-of-flightmass spectrometry (GC-TOFMS) is well-suitedfor investigating shelf stability applicationsbecause it provides non-targeted aromaprofile characterisation. Sensory analysis isalso common for shelf-stability and generalproduct quality applications. These arecomplementary analytical techniques andusing them together is beneficial.The sensory analysis provided overallfreshness and quality scores for each sample,while the non-targeted GC-MS analysisprovided comprehensive aroma profilechemical data.These data were mined for specific analytesof interest and were also reviewed to discoverinherent trends and differences in the aromaprofile that correlated with the sensoryanalysis results.Key Words# Beer# Shelf-Stability# Aroma Profile# Sensory Analysis# HS-SPME# GC-TOFMS# Deconvolution# PCAView Application NoteOverlaid chromatograms from all samples are shown. A plot showing the correlation of th sensory scores with the PC1 scores from the chemicalanalysis shows good agreement. The heat map highlights peak areas of analytes that correlate with sensory score.Instrument: LECO PEGASUS BT20 // LECO Food 2020

DISCOVERING THE SCENTOF CELERY HS-SPME, GC-TOFMS,AND RETENTION INDICESFOR THE CHARACTERISATIONOF VOLATILESDetermining and identifying individualanalytes within a complex sample canprovide important characterisationinformation for better understanding of asample, product, or process. This type ofexploratory analysis is readily accomplishedwith GC-TOFMS, as it provides non-targeteddata with every acquisition.The PEGASUS BT adds to thechromatographic separation by takingadvantage of the full mass range datawith mathematical deconvolution to furtherseparate chromatographic coelutions.The ChromaTOF software contains tools tohelp streamline data analysis. For example,retention index meth

Next Page LECO Corporation – company facts Selection of LECO SepSci App Notes LECO Food Testing Bibliography GC- and GC GC-TOFMS instrumentation Specific LECO GC-TOFMS . Cold Jet Hot Jet Stage 1 Hot Jet Stage 1 Cold J

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