CHROMATOGRAPHIC SPECIALTIES INCLife Science Products . Our sister company, MJS. BioLynx, offers...

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1-800-267-8103 Chromatographic Specialties Inc.

BRIEF INTRODUCTION — SAMPLE PREPARATION TECHNIQUES

Technical Support and Instrumentation Assistance Need expert advice? Our friendly and knowledgeable Technical Support and Instrumentation Teams consist of experienced chromatographers who understand the challenges facing separation scientists. They are available to assist you with everything from method reviews, to application support and troubleshooting.

Analytical Method Improvements• Takeadvantageofproductsthatcanpumpoutresultsinlesstime,whileconsuminglesssolvent and minimizing the need for retesting due to out-of-spec results• Manysamplepreparationtechniquescanbeautomatedtohelpsaveonlabourcostsandimprove consistency

$ It is estimated that 60-80% of the work done in an analytical lab is spent on sample preparation. We can help you increase your productivity and reduce costs.

Call UsOur receptionist, order desk, customer service and technical support departments, in fact our entire company, is staffed by real people. Are you tired of trying to negotiate your way through frustrating automatedvoicesystems?Callus!We’llbehappytohelpyou.

Samplepreparationplaysasignificantroleinthequalityofanalyticalresults;ithelpsensurethatsamplesareinasuitableformtobeeasilydetectedusingsimple,robustanalyticalmethods.Despitethis,weoftenputoureffortsintorefininganalyticalmethodsrather than improving the methodologies of gathering and preparing the sample itself.

Samplepreparationtechniquesclean,concentrateandifnecessary,modifytheanalytespriortoanalysis.Clean-upandconcen-trationstepsimprovesignal-to-noiseratios.Clean-upremovesinterferingmaterial,therebyloweringnoiselevels;italsohelpsto preserve columns and instrumentation parts by protecting them from contamination. Concentration steps increase the signal and detectability by increasing the amount of analyte present in a given volume of sample.

This handbook provides an overview of the various sample preparation techniques available; our goal in creating this brochure was to help our customers answer two questions: • CanIimprovemysamplepreparationmethodsforgreaterspeed,cleanlinessorconcentration?• Whattechniquesaremostlikelytobebeneficialtome?

Todoso,we’velaidoutthishandbookasfollows:•

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We encourage you to consider the techniques used in your laboratory. Should you wish to discuss your current sample preparationprocessesorinvestigatepotentialimprovements,pleasedonothesitatetocontactus.

Thefirst8pagesoverviewvarioussamplepreparationtechniquescommonlyusedintoday’slaboratories.Theyaregroupedbysamplematrix,goingfromliquid,throughsolidstogases.Thesepageshighlighttheprosandconsofeachtechniquevis-à-vistheothersandshouldhelpidentifywhichtechniquesaremostsuitableforyourlab.Wefollowthosewith4pagesofindustryspecificexamplesofchallenginganalyses.Onthosepages,weexplainthechallengethen provide an overview of the method used to address the issues. - Wehaveover500samplepreparationapplicationsavailable,spanningmanydifferenttypesofsamplesandtechniques. We’reconfidentwecanhelpyouimproveyourmethods.The last half of the handbook introduces products that CSI has available to address your sample preparation needs.

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TABLE OF CONTENTS

Overview of Sample Preparation Techniques ...........................................................................................................................4

Industry / Application Examples• MedicalMarijuanaApplication .......................................................................................................................................12• DrugTestingApplication ................................................................................................................................................13• FoodTestingApplication ................................................................................................................................................14• EnvironmentalTestingApplication .................................................................................................................................15

Product Overview• SolidPhaseExtraction(SPE) ........................................................................................................................................16• AutomatedSamplePreparation ....................................................................................................................................20• QuEChERS ...................................................................................................................................................................22• ColumnsforPhaseSeparation......................................................................................................................................24• SoxhletExtraction..........................................................................................................................................................25• Purge&Trap/ThermalDesorption ...............................................................................................................................26• All-in-OneGCAutosamplers .........................................................................................................................................27• SyringeFiltersandFilterVials .......................................................................................................................................28 • DerivatizationReagents ................................................................................................................................................30• SolidPhaseMicroextraction(SPME) ............................................................................................................................31

Wait! There’smore…We offer many more sample preparation products, as well as products for sample collection.

Propersamplecollectionalsoplaysanimportantroleinobtainingqualityresults.Contact us for more information.

Life Science Products Our sister company, MJS BioLynx, offers products for biological sample preparation. Visitwww.biolynx.ca or call 1-888-593-5969 for more information.

Greatideastohelpyouandyourlabreduce costs.

Tips and Tricks to help you get better results.

Save time so you can focus on other tasks or process more samples.

ThinkGreen! Help the environment by using less solvent or generating less waste.

$ Industryspecificexamplesofchallenginganalyses. Contact us for help with your specificapplication.

Freesamplesareavailableforcertainproducts. Contact us and try these products in your lab.

Contact our Technical and Instrumentation teams for more information or for assistance.

Throughoutthehandbook,lookforthesesymbols,they’llprovideinformationtoillustratehowwecanhelpyousavetime,moneyandeffort…

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4 1-800-267-8103 Chromatographic Specialties Inc.

OVERVIEW OF SAMPLE PREPARATION TECHNIQUES

Solvent ExtractionsClassicextractionmethodswhereanalytesareextractedintoaliquidsolvent,typicallyahighvolatilitynon-polarorganicsolvent.

Technique Advantages Disadvantages NotesLiquid-Liquid Extraction (LLE)

Sample Type: Liquid

Purpose: Removaloforganicanalytes from aqueoussolutions

Verybasicequipment

Tolerates very dirty samples

Labour intensive Large amount of solvents used

Solvent choices are limited to immiscible solvent pairs

Concentrates analytes (withadditionofsolventevaporationstep)

The extraction is most often performed in a separation funnel

Two immiscible solvents are shaken together, the analyte partitions into its preferred solvent

Competingtechniques:SPE,SLE,SPME

Supported Liquid-Liquid Extraction (SLE)

Sample Type: Liquid

Purpose: Removaloforganicanalytes from aqueoussolutions

FasterthanLLE,eliminates emulsions, lowers solvent consumption

Offers some advantagesofSPEwithoutrequiringfullmethod development

LessspecificthanSPE Volumeofsamplefor extraction is very limited compared to eitherLLEorSPE

ModificationofLLE

Aqueoussampleis adsorbed on diatomaceous earth, then extracted by passing immiscible organic solvent over sorbed sample

Competingtechniques:LLE,SPE

Solid Phase Extraction (SPE) Sample Type: Solidsandliquids Purpose: Removalofimpuritiesand concentration of analytes

ComparedtoLLE: Saves time and money

Uses less solvent

Achieves better recovery and cleaner samples to better protect instrumentation Can be automated Broader applicability thanSPME

SlowerthanSPMEforSPME-appropriatesamples

A sorbent is used to extract analytes of interest

Solvents of different polarity are used to wash, condition and ultimately separate the analytes of interest from interfering compounds Competingtechniques:LLE,SLE,SPME See page 16

Technical SupportNeed expert advice? Our friendly and knowledgeable Technical Support and Instrumentation Teams consist of experienced chromatographers who understand the challenges facing separation scientists. They are available to assist you with everything from method reviews, to application support and troubleshooting.Thisisafreeserviceforourcustomers;wewillnotchargeforhelpingyouresolveachromatography problem.

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Technique Advantages Disadvantages NotesDispersive SPE (dSPE) Sample Type: Solidsandliquids Purpose: Removalofimpurities

FasterthancolumnSPE

Not as thorough ascolumnSPE

SPEpackingmaterialisadded directly to a solu-tion rather than passing it through the packed mate-rial in a cartridge or tube

TheSPEsorbentis removed by centrifugation orfiltration

Competingtechniques:columnSPE

QuEChERS Sample Type: Solidsandliquids

Suited for pesticide extracts in foods and similar products such asmarijuana,wines,cooking oil, soils, etc.

Purpose: Removalofimpuritiesand concentration of analytes

Fasterandlower solvent use than Soxhlet

Uses lower toxicity solvents Works better with physically dirty samplesthanPLE

Less automated thanPLE

QuEChERSstandsforQuick,Easy,Cheap, Effective,Rugged,Safe

Involvestwosteps:

1)Saltingoutextraction using buffered or unbuffered solvent (usuallyacetonitrile)

2)DispersiveSPE(dSPE)in which solid adsorbent isusedtotreatanaliquotfrom step 1 to remove interferences

Ideal for selective detectors suchasMS

Competingtechniques:Soxhlet,PLE

See page 22

Soxhlet Extraction

Sample Type: Solids

Purpose: Removaland concentration of organicanalytes(withaddition of solvent evaporationstep)

Onlybasicequipmentrequired

Slow

Requireslargevolumes of organic solvents

Requirescontinuousflowofcoolingwater

Solventisrefluxedthroughthe sample, which is held in a porous thimble

Analytes of interest are collected and concentrated in an organic solvent

Competingtechniques:PressurizedLiquid Extraction(PLE), QuEChERS

See page 25


SolventExtractions(Cont’d)

Choosing between dispersive and column SPEDispersiveSPEisafasttechniquetoremovegrossimpuritiesfromyoursample.Asthesorbentsaresimplymixedintoaliquidsamplethenremovedbycentrifugationthetechniqueisveryfastandrequiresalmostnooperatorattention,butitonlyhasanadsorptionstep,limitingitsselectivity.ColumnSPEaddswashingandselectiveelution,socontaminantsthatarebothmoreandlessattractedtothesolidphasethanistheanalyteareremoved.However,itisslowerandcanrequiremoreoperatorattention.

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SolventExtractions(Cont’d)

Technique Advantages Disadvantages NotesPressurized Liquid Extraction (PLE) Sample Type: Solids

Purpose: Removaland concentration of organic analytes

Fast Reproducible Automated

Requireslarge capital investment

Pressurevesselsneed to be cleaned beforereuse(notpractical to use disposablevessels) Particlebreakthroughcan damage expensiveequipment

Organic solvent is applied to the sample at high pressure and temperature(above normalboilingpoint)

Competingtechniques:Soxhlet,QuEChERS

ConcentrationConcentration is usually done after solvent extraction. The extracting solvent is evaporated off, leaving the less volatile analytes concentrated in a small volume of solvent. It can be taken to the extreme of evaporating all the original solvent and replacing it withamorepolar(lessvolatile)solventinsolventexchange.

Kuderna Danish Sample Type: Extracts

Purpose: Concentration after extractiontoliquidphase

Best recovery of volatile compound duetorefluxaction

Can process 6-12 samples at a time

Time consuming Startvolume:500mL

Endvolume:0.5mL

Hybrid Evaporation

Sample Type: Extract

Purpose:Concentration after extractiontoliquidphase

Handles large and small samples Goodrecoveryevenonvolatile compounds

Moderatespeed

Built in drying system

Total automation

Moreexpensivethan using a single method

Startvolume:upto200mL Endvolume:directlyinvialdown to 500 µL Combines vacuum, blowdown and Kuderna Danish

Rotary Evaporator

Sample Type: Extracts


Handles large samples

Concentrates individual samplesquickly

Volatilecomponentstend to have medium recovery

Finalvolumeoftentoo high for analysis, requiringsecondaryevaporation

Can process only one sample at a time

Startvolume:upto1L

Endvolume:5to10mL(includingrinses)

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Concentration(Cont’d)

Technique Advantages Disadvantages NotesNitrogen Blowdown

Sample Type: Extracts


Can process up to 60 samples at a time

Can accommodate a variety of sample sizes

Low recovery of volatile compounds

Higher running costs due to gas consumption

Usually all samples must be in the same size tube

Evaporationslowsdown later in run unless pressure is raised

Startvolume:1to200mL

Endvolume:0.2to0.5mL

See page 21

Dialysis

Sample Type: Liquids,Proteins

Purpose: Contamination removal and desalting

Simple and easy to set-up

Gentle

Low cost

Slow

Lackofspecificity

Exchangeofbuffermediumacross a semi-permeable membrane

New dialysis tubes incorporate dialysis membrane in cap to reduce sample loss

Extraction to Sorbent PhaseExtractionstosorbentphasesdependonpartitioningbetweenaliquidorgasphaseandsolidorbonded“pseudo-liquid”phasetoseparateandconcentrateanalytes.Followingadsorption(toasolid)orabsorption(inapseudo-liquid),eitherthesurroundingsolventorthetemperatureischangedtodrivetheanalytesintothefinalphaseforanalysis.

Solid Phase Microextraction (SPME) Sample Type: Liquids,gasesandheadspace over solidsorliquids Purpose: Concentration of analytes

Fastandclean Largely limited to volatile or semi-volatile compounds

Fusedsilicafiberiscoatedwith polymeric stationary phase

Analytes diffuse and partition/adsorbontostationary phase

Analytes are then thermally desorbedbyplacingfiberintoGCinjectionport Competingtechniques:PLE,LLE,SPE

See page 31

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Instrumentation SupportOurInstrumentationTeamisavailabletoansweryourquestionsandperformcalibrationsandrepairstoyourinstrumentation.Theycanalsocustomizeinstruments,andperformdifficultmodificationsandinstallationstofityourspecificapplicationsorneeds.

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ExtractiontoSorbentPhase(cont’d)

Technique Advantages Disadvantages NotesThermal Desorption Sample Type: Volatilesinsolids, liquidsoringasphase

Purpose: Extractionandcon-centration of volatile organic compounds (VOCs)

Allows for trace level analysis

Nosolventsrequired

Extractionand concentration in one step

Little to no sample handling

CleanGCinjection

Strictly for volatiles

Requiresspecificinstrumentation

Samples are pumped through a sorbent material (Trap).TrappedvolatilesarethendesorbedtoGC orGC/MS. Withspecialequipment,near real-time monitoring can be performed Competingtechniques:Bulk sampling bags or sample canisters

See page 26

Purge and Trap - Dynamic Headspace Sample Type: Volatilesinliquid or solid samples

Purpose: Forextractingandconcentrating volatile organic compounds (VOCs)fromliquids and solids

Allows for trace level analysis

Nosolventsrequired



CleanerGCinjection


Limited sample size (forpurgeandtrap)

Requiresspecificinstrumentation

Samples are purged with inert gas to drive volatiles to a sorbent material(Trap).Trappedvolatiles are then desorbed toGCorGC/MS. Withspecialequipment, Dynamic Headspace can be performed on large objects

Competingtechniques:SolidPhaseMicro Extraction,StaticHead-space

See page 26

Static Headspace

Static Headspace Sample Type: Volatilesinliquid,solidor mixed matrices

Pharma,food, and biological

Purpose: ExtractionofVOCsfrom complex matrices

Nosolventsrequired



CleanerGCinjection


Limited sample size

Typicallyrequiresspecific instrumentation

Volatilesareforcedfromthe matrix to attain an equilibriumbetweenphases

Heat, agitation and time are used to drive the equilibrium

Competingtechniques:SolidPhaseMicro Extraction,Purge&Trap

See page 27

Whenanalytesarevolatileandthesolventis(relatively)non-volatile,heatingaclosedvesselconcentratestheanalytesinthegasphaseabovealiquidorsolidsample.Samplingthishead-spacewithagas-tightsyringeallowsasimpletransferofthedesiredvolatilecompoundstoaGC,whileeliminatinganyrelativelynon-volatilecompoundswhichwouldotherwiseaccumulateintheGCinletandtheheadoftheGCcolumn.

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Supercritical Fluid Extraction (SFE) Amodernrevisionofsolventextraction,SFEreplacesorganicsolventswithsupercriticalfluids.Astheyareneithergassesnorliquids,theviscosityanddensityofsupercriticalfluidscanbecontrolledoversignificantrangestoallowbetter,fasterextractions.

Technique Advantages Disadvantages NotesSupercritical Fluid Extraction (SFE) Sample Type: Bulk plant materials

Purpose: Extractionfromsolids

Uses inexpensive, non-toxic solvents

Fast

Automatable

High cost of equipment

Limited selectivity

Sample is placed in a flow-throughcolumnandsupercriticalfluid(typicallyCO2)ispassedthroughthe sample. The density and viscosity of CO2 can be controlled. The extracted analyte is collected in solvent or trapped on adsorbent. Collecting pure analyte is simple as CO2 returns to gas under ambient conditions

Automated and manual versions available Competingtechniques:Quechers,Soxhlet,PLC

Particle Removal Solidparticlesinaliquidsamplecanpluganderodesensitiveinstruments.Thesetechniquesperformsimplephysicalseparationsto eliminate particles of all types.

Filtration Sample Type: Liquid

Purpose: Particleremovalor concentration of particles as a solid sample

Cleaner product than centrifugation

Handles larger volume samples than centrifugation orsyringefiltration Helps extend column and instrument life No effect on dissolved chemical contaminants

Handles fewer samples at a time than centrifugation

Doesn’thandlesmallvolume samples well

Somefiltersworkwithgravityflow Finerfiltersrequiresupportand vacuum for reasonable speed Competingtechniques:Syringefiltration, centrifugation

Syringe Filtration

Sample Type: Liquid Purpose: Particleremoval

Cleaner product than centrifugation

Better than standard filtrationforsmallsamples

Handles fewer samples at a time than centrifugation

Doesn’thandlelargevolume samples well

Attaches to luer or luer lock syringe

Syringe provides pressure forfasterfiltration Competingtechniques:filtration,centrifugation,spinfiltration

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OVERVIEW OF SAMPLE PREPARATION TECHNIQUESParticleRemoval(Cont’d)

Technique Advantages Disadvantages NotesSpin Filtration

Sample Type: Liquid

Purpose: Removeparticles fromliquidsamples

Cleaner product than pure centrifugation

Better than standard filtrationforsmallsamples

Handles batches of samples

Doesn’thandlelargevolume samples well

Relativelyexpensivedue to cost of centrifuge

Centrifugal force is used topressliquidthroughmembranefilter

See page 23

Centrifugation Sample Type: Liquid Purpose: Separation of substances with different densities

If the tubes are reused, the process may be less expensive

Less interaction between sample andvariousfilter membranes

Can be a slow process

Relativelyexpensivedue to cost of centrifuge

Uses centrifugal force to separate 2 or more components in a mixture or suspension Samples are placed in specialtytubes(disposableorreusable)andspunathigh speeds to create a separation

Competingtechniques:Syringe, membrane and paperfiltration

Derivatization DerivatizationchemicallymodifiesanalytestoimprovevolatilityforGCseparationsortoincreasetheirUVabsorptionor fluorescenceforLCdetection.Bothcanmakeanalytesmorevisibleinananalysiswithoutincreasingconcentrations.

Derivatization Sample Type: Liquidorsolid Purpose: Alteration of difficult-to-analyzesamples to make them more visible to GCorLCdetectors

Providesincreasedsample volatility Improved selectivity

Enhanceddetectability

Reagentsare often moisture or air sensitive

Residuesbuildup inGCdetectors

Reagentsoften harmfultoGC column phases

Generally,threemethodsofderivatization:Silylation,Acylation and Alkylation

Competingtechniques: in some cases, pyrolysis + FT-IRoranother spectroscopy method

See page 30

Our Technical Team is only a call away!

ContactusformoreinformationonSamplePreparationTechniques.

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Precipitation Precipitationchangesthechemicalconditionsinasampletocauseundesiredsolutestoprecipitateout,foreasyremovalby filtrationorcentrifugation.Itisoftenusedtoremoveproteins,butcanalsoworkforsalts.

Technique Advantages Disadvantages NotesProtein Precipitation

Sample Type: Serum, plasma, otherbodilyfluids

Purpose: Bulk removal of proteins

Quick,inexpensiveprotein removal

Precipitatedproteinscan trap analytes

Addition of organic solvent can make injectionsolventtoostronginRPHPLC

Adding polar organic solvent(acetonitrile,methanol)tosample denatures proteins, causing precipitation

Precipitateisremoved byfiltration

Also known as protein crash

Immunoprecipitation

Sample Type: Cell or tissue lysates

Purpose: Enrichmentof specificproteins

Highlyspecificfordesired proteins

Elutioncan sometimes result in low protein recovery and antibody contamination

Can be used to remove high abundance protein in order to analyze low abundance proteins

AffinityChromatography Affinitychromatographyinvolvestheremoval(orinsomecasesconcentration)ofanalytesbyantibody–antigeninteractions. Thistechniqueoriginally,andstilllargely,usesmonoclonalorpolyclonalantibodies;however,someanalytescannowbetargetedby specially synthesised polymers with tailored molecular level pockets.

Affinity Chromatography

Sample Type: Bodilyfluids,cellortissue lysates

Purpose: Enrichmentof specificproteins

Highlyspecific

High recovery for small volume samples

Elutioncan sometimes result in low protein recovery and antibody contamination

Requirescolumn derivatized with suitable antibodies

Can be used to remove high abundance protein in order to analyze low abundance proteins

Sample Prep Automation $Despitetheinitialcostoftheinstrumentationandthelabourinvestmentneededtointegratethesystemintotheworkflow,thebenefits(increasedturnaroundtime,highsamplethroughput,betterconsistencyanddecreasedneedforre-analysis)leadtoaverygoodreturnoninvestment.Inmostcases,thepaybackperiodisbetween9-18months,allowingyourcompanytolowerthecostofeachanalysisforextraprofitorgreatercompetitiveness.

Contact us for a

a Minimize human error and increase reproducibility a Reduce hands-on time so you can focus on other tasks

Process more samples in less time

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MEDICAL MARIJUANA APPLICATION

Marijuanaediblesareparticularlydifficultsamplestoanalyse, both for forensic labs assessing seized products and for licensed medical marijuana producers. Fats and sugars included in edibles are notori-ous for contaminating instruments and columns.

Procedure: (Abbreviatedmethod.Contactusforfulldetails.)

1. Sample Homogenization: (similar processing is used for all extraction techniques) • HardCandiesandChocolates-groundtoafinepowder using a freezer mill. • GummyCandies-cutintoslimpieces. • CarbonatedBeverages-degasfor30min by sonication.

2. QuEChERS Extraction <2min/sampleand<90min/batch,<15min/batchforcarbonated

beverages. a. Carbonatedbeverages:Toa50mLcentrifugetubeadd10mL of the degassed sample and internal standard.

Candies,bakedgoods,oroil:Toa50mLcentrifugetubeadd1gofthepre-treatedsamples,internalstandardand 10mL of reagent water. Hydrate for 1 hour using a horizontal shaker.

b. Add10mLofacetonitrile(MeCN)with1%aceticacid. c. AddQuEChERSextractionsaltsfrompouches(Product#UCTECQUUS950CTMP),andvortexfor10seconds. d. Shakevigorouslyfor1minute.Forgummysamples,add2metalballsandshakefor10minutes. e. Centrifuge for 5 minutes.

3. Dispersive SPE Clean-up for Pesticide Residue Analysis <2min/sampleand<10min/batch a. Transfer1mLofthesupernatantto2mLcentrifugetubepre-loadedwithdSPEsorbents Product#UCTECQUUS142CT) b. Shakevigorouslyfor1minute;centrifugefor5minutes. c. Vortex200µLextractwith200µLofDIwaterina2mLvialfor30seconds;inject.

4. Serial Dilutions for Cannabinoid Analysis a. DiluteQuEChERSextractsto100to200ng/mLofcannabinoidsbasedonexpectedconcentrations. b. Spikethedilutedsampleswithtargetcannabinoids;quantifyusingthestandardadditionmethod.

Ready for analysis of pesticide residues and potency in approximately 2 hours.

Fast, proven, sample clean-up for pesticides and cannabinoids in marijuana edibles.

QuEChERS is:

• Aneffectivemethodforfastreductionofmultiplecontaminantclassesfromsamples.• A“just-enough”technique:captureanalytesassoonasjustenoughclean-upisdoneforsimpleanalysis.• Abroadlyuseabletechniqueformanyclassesofanalytes.• Applicabletomanyformatsofnaturalhealthproductsorfunctionalfoods.Assesssafetyandefficacywithoneclean-up.

Application ExampleContact us for help with yourspecificapplication.

The techniques outlined here can be applied to other foods or to activecompoundsinNaturalHealthProducts.

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DRUG TESTING APPLICATION

Drying columns between steps allows immiscible solvents to be used in succes-sive steps. If miscible solvents are used, no drying is needed. This is an advantage over LLE: you can usemiscible solventswithoutriskofnon-specificextractions.

Save time on sample prep – conditionyour columns while centrifuging your tissue samples!

Advantages of CLEAN SCREEN® DAU and other Copolymeric SPE Phases:• Thoroughremovalofmultiplecontaminantclassessuchasprotein,fats,andsugarsthroughhighspecificityandbroadretention. Reversedphaseandionexchangemechanisms,twowaystoretainanalytesorcontamination. Visitwww.chromspec.com/spe-app for examples of different extractions.• Excellentloadingandretention. Both phases are on every particle, minimal analyte movement when changing retention mechanisms.

Clean-Screen DAU is optimized for general drugs of abuse. Contact us for other special or general purpose copolymeric phases.


Copolymeric SPE Column Extraction of Barbiturates from Body Fluids or Tissue Bodilyfluidsandtissuesarechallengingmatricestoanalyze. Proteins,fats,sugarsandsaltswillallbepresenttosomedegree, and can all interfere with GC or HPLC analysis.


1. Prepare for Extraction: <2minsampleofhandling,15minutes/batchnonoperatortime a. Mix1mLof100mMphosphatebuffer(pH6.0),internalstandards and1-2mLofblood,plasma/serum,urine,or1ghomogenisedtissue. Mixvigourouslyandletstandfor5minutes. b. Add2mLof100mMphosphatebuffer(pH6.0).Mixvigourously. c. SamplepHshouldbe6.0±0.5,adjustpHsodiumphosphateifneeded. d. Centrifuge for 10 minutes at 2000 rpm and discard pellet.

2. Condition CLEAN SCREEN® Extraction Column: Approximately2minutes/24columnbatch (Product#UCTZSDAU020.Thesteppedtubedesignconcentrates moresampleonlessstationaryphase.) a. 1 x 3 mL CH3OH b. 1 x 3 mL D.I. H2O c. 1x3mL100mMphosphatebuffer(pH6.0) NOTE:Aspirateatfullvacuumorpressure.

3. Apply Sample to Column: 1.5-3 minutes per batch of 24 columns a. Poursupernatantfromstep1ontopoffreshlyconditionedcolumn. b. Aspiratethroughcolumnat1to2mL/minute.

4. Wash Column: 10 minutes per batch of 24 columns a. 1 x 3 mL D.I. H2O b. 1x1mL100mMAceticAcid c. Drycolumn(5minutesatfullvacuumorpressure). d. 1 x 2 mL hexane

5. Elute Barbiturates: 1.5-3 minutes per batch of 24 columns a. 1x3mLEthylAcetate:Hexane(50:50) b. Collecteluateat1to2mL/minute.

6. Dry Eluate: Time depends on available dry down tools a. Evaporatetodrynessat<40°C.

7. Reconstitute / Derivatize: 2minutes/batch a. LC-MS/MS:Reconstitutesamplein100µLofmobilephase;inject10µL. b. GC-MS: Dissolveresiduein100µLofEthylAcetate. OptionalDerivatizationforIncreasedVolatility. AlkylatewithTMPAH(ReactionoccursinGCinjectionport!Noaddedtime).

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FOOD TESTING APPLICATION

Column SPE/QuEChERS Procedure for Analysis of Bisphenol A in Canned Food Products

WithcolumnSPE,differentphasescan be run in series or different clean-up steps can be run simulta-neously by using column adapters to stack columns on top of each other as they go through a vacuum manifold.


1. QuEChERS Extraction <2minutes/sampleand5minutes/batchforcentrifugation a) Addweighedsampleandinternalstandardtoa50mL QuEChERStube b) Add10mLofacetonitrileandmix c) SaltoutacetonitrilefromwaterwithQuEChERSsaltmix (Product#UCTECQUEU750CTMP) d) Shakevigorouslyfor2min.andcentrifugefor3min.

2.1. Column SPE Clean-up for Lightly Pigmented Food <10minutes–PSAandC18forlipidremoval a) AttachProduct#UCTECPSAC1856tothevacuummanifold and add Na2SO4(Product#UCTECSS10K) b) Conditionwith2x2mLofacetonitrile c) Loadthesupernatantandcollecttheextract d) Concentratetodryness

2.2 Column SPE Clean-up for Highly Pigmented Food <10minutes–PSAandGCBforlipidandpigmentremoval a) AttachProduct#UCTECPSACB6tothevacuummanifold and follow the same steps as 2.1

3. Derivatization and Analysis a) Reconstituteandsilylate;analyzebyGC/MS. Forinformationonderivatization,includingsilylation, reagents and their uses, please see page 30 or visit www.chromspec.com/derivatization

Humans put the “omni” in omnivorous, our foodsmay be animalor vegetable, fatty or lean, full of pigments or nearly white. Thismakesextractionandcleanupfromfoodsaparticularchallenge,butQuEChERS can handle all of these conditions.

QuEChERSisaflexibletechnique

QuEChERSnormallyusesdSPEforgreaterspeed.However,withchallengingmatricessuchaspreparedfoodswithmultipleingredients,columnSPEcanbeusedformoreeffectiveclean-up.ThisflexibilityhasallowedQuEChERStoevolvefromatechniqueforfruitsandvegetables,meatsandseafood,toincludesoilsamplesandevenproductssuchasbabytoys.

Visitwww.chromspec.com/quechers for more information.


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ENVIRONMENTAL TESTING APPLICATION

Extraction and Sample Concentration from Large Volumes of Water

1/8” OD PTFE tubing and an appropriatecolumn adapter allow you to extract water samples ranging in volumes from hundreds of millilitres to liters straight from the sampling bottle.

Column SPE and transfer lines provide you with:

• Simple,reliableextractionoflargevolumesofwaterwithminimaloperatortime

• A50:1concentrationstepoccursbefore sample blowdown! (Comparedtotypical5:1concentrationswithLLE) -Forsomecompounds,extractioncanprovideanevengreaterconcentrationratio. -Final10:1concentrationisfromjust20mLofsolvent.

• Flexibilitytousewatermisciblesolventstoextractpolarorganicsfromwatersamples.

Visitwww.chromspec.com/spe-app for more information.

Thisanalysisconcentratespesticides500:1fromwatersamples.


EPAMethod8141B-DeterminationofOrganophosphorusPesticidesandTriazineHerbicidesinWaterbySolidPhaseExtraction.

1. Sample Spiking a. Add surrogate standard to 1L portions of neutral water samples (Note:useofsmallersamplevolumesispermittedifmethodsensitivityisnotanissue).

2. SPE Cartridge Conditioning a. WashtheSPEcartridgeswith3x5mLDCM b. Condition cartridges with 2 x 5mL methanol. c. Equilibratethecartridgeswith2x5mLDIwater.

3. Sample Loading a. ConnectwaterreservoirstoSPEcartridgeswithtransferlines.Drawsamplesthroughinafastdrop-wisefashion (10-15mL/minute). b. Removethetransferlines,drycartridgesundervacuumfor10minutes.

4. Eluate Drying and Elution a. AttachthedryingcartridgesbelowSPEcartridges,placecollectionvialsinmanifold. b. Rinsebottle,transfertube,eluteSPEcartridgewith5mLacetone,10mLDCM. c. Removethetransfertubes,eluteSPEcartridgeswith5mLDCM.

5. Eluate Concentration a. Concentratetheeluatestoabout0.5mLunderagentlestreamofnitrogenat40°C. b. Rinsewallsofvialswith3mLofn-hexane,concentratetoabout2mL. c. Transfertheextractsto2mLvials,adjustthevolumeto2mLwithn-hexane. d. Addinternalstandard,samplesarereadyforGCanalysis.

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SOLID PHASE EXTRACTION (SPE)

SPEcolumnsareidealforlaboratoryextractionswhenavacuumorpositivepressuremanifoldorSPEautosamplerisavailable.Theirminimalistdesigncutscostandwaste,and allows for easy packing to suit all needs.

SPEcolumnsaremadeofpolypropyleneorglass,areavailableinavarietyofshapesand have volumes of approximately 1mL to 50mL. Columns may be attached in series orwithlargevolumereservoirs,usingadapterfittings.Acertainweightofsorbentma-terial is contained in the column between an upper and lower frit. They are primarily used with vacuum or positive pressure manifolds to move samples through the column. Automatedsystemsareavailable(seepage20).

SPE Columnsa Aflexible,reliable,costeffectivesolutionforlaboratoryextractions

SPE Formats

SPEisanextremelypowerfulandflexiblewaytoconcentrateandpurifyanalytesofinterestandremovecontaminantsfromsamplematrices.SPEproductshavebeendevelopedforspecificapplicationsusingawiderangeofsorbents,formatsandsizes.Here,weprovideabriefintroductiontoselectingfromthesedifferentSPEproducts.

Formoreinformation,pleasecontactourTechnicalteam.

Using SPE instead of LLE can save you time and money

• Fasterprocessingwithfewerstepsandlesssamplehandling• Useslesssolventandglassware• Doesnotrequiretheuseofimmisciblesolvents,simplifyingsolventselection• Greateranalyterecoveries,soyoucanworkwithsmallersamples• Lowerriskofcrosscontamination• Highlyreproducibleextractionsforbetterresults• Morespecificextractsforbetterequipmentprotection• Createslessdisposablewaste,whichhelpstheenvironment

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TheUCTSPEColumnlineincludesproductsspecificallydesignedforusein:

• Clinical and Forensic – fortheextractionofacids,neutralsandbases;idealforbothscreeningandconfirmationanalysesof virtually all drug categories

• Environmental–widerangeofcartridgesizes,sorbenttypestailoredtothespecificrequirementsofeachanalysis

• Toxicology–extractawidearrayofbasicdrugsincludingbenzodiazepines,opiatesandTHCmetabolite

• General Sample Clean-up–ofpolar,non-polarandioniccompounds

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Push-Thru Cartridgesa Excellentforfieldsamplingandavoidingcarryover

Withluerconnectorsatthetopandbottomofeachunit,Push-Thrucartridgesallowsamplestobeloaded,washed,orelutedusingasimpleluertipsyringe.Justslipthesyringe into the female luer inlet of the cartridge and push sample through with the syringe.

Youcanchoosefromawiderangeofsorbent typestailoredtothespecificrequire-mentsofeachanalysis.Excellentforfieldsampling,andavoidingcarryover.Canbeused with vacuum manifolds if needed.

TheUCTPush-ThruCartridgelineincludesproductsspecificallydesignedforusein:

• Environmental–Captureandconcentratefieldsampleswithlightweightanddurableequipment.Transportingsamplesorbed toSPEphaseeliminatesweight,chanceofspills,andcanprovideadditionalstability.UCT’sspecialtyGlyphosatePush-Thru cartridgesstripcommonmatrixcomponentsinterferingwithglyphosateionisationanddetectioninLC/MS.

• ClinicalandForensic–Push-Thrucartridgescombinedwithstandarddisposablesyringesprovideasimpleinexpensivesingle useflow-pathatthesamplecollectionpoint.

• GeneralSampleClean-up–Avoidtyingupvacuummanifoldsorautomatedextractorsformethoddevelopmentandproofof conceptforSPE.Testmethodsonsinglesamplesatthebenchwithasyringeandcartridge.

Extraction Disksa An ideal solution for large volume samples

Thediskformatprovidesalargesurfaceareaforsorbent/samplecontact.Fasterflowratesandhigherthroughputarerealizedcomparedtoliquid-liquidextractionortradition-al packed column technology. The particle-loaded membranes, or disks, are produced using the most common sorbent particles. They provide a more uniform extraction mediumthancanbeachievedinatraditionalSPEcolumnorcartridgepreparedwiththesamesizeparticles.Extractionaccessoriesincludeamanifoldwithreservoir,disksupportandsuitablecollectionvials.Automatedsystemsareavailable(seepage21).

The3MEmpore™andHorizondisklinesfeatureproductsspecificallydesignedforusein:

• Environmental–Forfastextractionsoflargewatervolumes.Commonanalytesofinterestarepersistentorganicpollutantsin surfacewatersortracesofoilandgreaseinwastewater(EPA1164).

Productsinclude: • Reversephase • MetalScavengers • Ionexchange • ActivatedCarbon • OilandGrease • Pre-filtersforparticleladensamples

Symptoms of a Sample in Need of Further Clean-up:• Poorreproducibility• Columnfailure(highbackpressure,changingretentiontimes)• IncorrectquantitationonQCsamples

FixingInsufficientlyCleanSamples:• Tryadifferentsorbentwhichusesthesameretentionmechanism (i.e.tryendcappedsilicaC18insteadofnon-endcappedC18)• Changetoadifferentretentionmechanismsorbent• Changethewashsolvent• Changetheionicstrength(whenusingionexchangesorbents)• ChangethepHoftheloadandwash• Changethe%organicoftheloadandwash• ContactourTechnicalSupportTeamtodiscussyourapplicationandcurrentmethod

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SPE Sorbents• SPEsupportsaremostlybasedonporoussilicaorpolystyrene-divinylbenzene(PSDVB)particles,withorwithoutderivatization• Particlesaretypically45-60µmindiameter,butmaybesmallerorlargerforspecificmethods• Particlesaretypicallyirregular,butmaybesphericalforcertainhighperformanceapplications - Large,irregularparticlesareveryeffectiveinSPE.Retentionisbinary(100%retained,or100%eluted),sothereislittleneed for high plate counts• MaterialsotherthansilicaorPSDVB(e.g.Florisilorgraphitizedcarbon)arealsoused,mostlywithoutderivatization

Hydrophobic (Reverse Phase) Extraction Sorbents • Sorbentiscomposedofnon-polarmoleculesbondedtosupportparticles.PSDVBmaybeusedunderivatized• Usedtoextractnon-polar/neutralcompoundsoutofcomplexmatrices• C18phaseisthemostwidelyusedbecausehighlypredictablehydrophobicretention• Analytesareelutedwithrelativelynon-polarsolventsystems• Commonphases:C18,C8,Styrene-DivinylBenzene(SDVB)

Hydrophilic (Normal Phase) Extraction Sorbents • Sorbentiscomposedofpolarorganicmoleculesbondedtosupportparticles.Silica,fluorisilandotherinorganicparticlesmaybe used underivatized• Compoundsareretainedthroughpolarinteractionse.g.hydrogenbonding,pi-piordipole-dipole.• Analytesareelutedwithrelativelypolar,sometimesaqueoussolventsystems• Commonphases:Silica,Fluorisil,Cyano

Carbon,GraphitizedNon-porousSorbents • Carbon can isolate extremely polar organic compounds• Carbonadsorptioncombineshydrophobicmechanisms,highsurfaceareaandionexchange• Thisinteractioncanhappeninawiderangeofpolarandnon-polarsolvents

Ion Exchange Sorbents • Sorbentmustcarryoppositechargetoanalyte.• Sorbentandtheanalytemustbeionizedforretention• Sorbentorcompoundmustbeneutralforelution• Sorbentiscomposedoforganicacidsorbasesbondedtoparticles - AnionExchangersincludeAminopropyl,QuaternaryamineandPolyamine - CationExchangersincludeCarboxylicAcid,BenzenesulfonicAcidandTriaceticacid

When pH is within 2 units of pKa acids and bases are in a mix of ionizedandneutralformleadingtoirregularretention/elution.

Cation AnionpH < pKa-2 + 0

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Sorbent Selection Considerations

• Doestheanalyteappeartobepolarornonpolar?• Aretheanalytessolubleinthematrix(andeluent)?• Dotheanalytescontainanyionicgroups?• Whatistheconcentrationoftheanalyteinthesample?• Arethecompoundsstableinacidorbase?• AreyouderivatizingforGCorHPLCanalysis?

Theanswerstothesequestionswillhelpdeterminewhichclean-uptechniquesorproductsmightworkfor your particular application.

Contact our Technical Support Team for further discussion.

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EXPERTADVICE




FREE SAMPLES are available!

Mixed Sorbents • Mixedchemistryisbeneficialwhenlookingtoextractbothaneutralandachargedcompoundoramphotericmoleculesfrompolar and non-polar molecules• Copolymericmixedsorbentsarecomposedoftypesofmultiplefunctionalchainsbondedtotheparticle.Oneionexchangeror polar chain, one hydrophobic carbon chain - Producedwithequalpartsofeachfunctionalgroupbondedtotheparticle - Yields reproducible bonded phases and allows the maximum use of mixed mode separation mechanisms• Mixedbedsystemshaveonephaseonanygivenparticle,mixtheparticlesfordualretentionmodes

Covalent Extraction Sorbents• Idealforscavengingreactivecompoundsinsyntheticchemistry• Covalentsorbentshaveeitherepoxy,aldehyde,isocyanateorthiopropylfunctionalgroupsthatareboundtothesilicabackbone by a hydrocarbon chain• Thesegroupsreactselectivelywithanalytefunctionalgroupscreatingapermanentchemicalbondbetweenthestationarysupport and the analyte

Visitwww.chromspec.com/spe for more information.

WeofferSPEproductsfromthesetrustedsuppliers:

Free Catalogue!GettheUCTSolidPhaseExtractionProductscatalogue.

RequestLiteratureCodeUCT27

3M Empore™

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Flexible,Precise,Modular

TheFREESTYLE™ is a fully automated sample preparation system for the unsupervised processing of food, animal feed, and pharmaceutical samples.

TheFREESTYLE™BASICbaseunitcanbeexpandedwithsomeorallofthefollowingmodules:• SPE Module–forSolidPhaseExtractionusingcolumnsbetween1mLand15mL• EVAporation Module–forevaporationorsolventexchange• GPC Module–forGelPermeationChromatographyofsampleswithcomplexmatrices• ThermELUTE Module–formycotoxinsamples,thisuniquemodulecanbeintegratedwithanyHPLCfora100-fold increase in sensitivity

When several modules are installed, each unit can be utilized individually or in combination.

AUTOMATED SAMPLE PREPARATION

Whychooseanautomatedsystem?$ • Processmoresamplesinlesstime• Minimizehumanerrorandincreasereproducibility• Reducehands-ontimesoyoucanfocusonothertasks

Designed for sample preparation for dioxin analyses, this system can be used for food, animal feed, and environmental samples.

• Fastprocessing:purifyyoursamplein50to60minutes• Lowsolventconsumption:300to400mLpersample

DevelopedincollaborationwithaleadinglaboratoryfordioxinanalysisinGermany,theCVUAMünster(Prof.Fürst/Dr.Bernsmann).

LCTech FREESTYLE™ a

Mycotoxins and Small Samples

LCTech DEXtech™

a Dioxin Samples

GPCModule

ThermEluteModule

SPEModule

EVAporationModule

Contact us for a FREE consultation and a Return on Investment calculation.

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AUTOMATED SAMPLE PREPARATION

Automated Solid Phase Extraction

• Programmableandmultipurpose–worksonawiderange of applications and sample types • Uses47mmdisks,90mmdisks,orstandardcartridges• Processessamplesdirectlyfromtheiroriginalcontainer• Automaticallyrinsesthesamplecontainer• PreconditionsthesorbentmaterialwithintheSPEdisk, passes the water sample through the disk, and elutes the sorbed analytes from the disk into a collection vessel

Total Walk-away Automation

• Positivepressurecontrolledvia6mLsyringe• Modularandscalable—upto8modulesfromonePC• Processupto12samplessequentially• Collectupto4fractionspersample• Workswithmostcartridgesizes(1,3,or6mL)• Independentmethodscanbeappliedtoeachsample

Horizon SPE-DEX® 4790a

For large volume or dirty samples

Horizon SmartPrep® Extractora

For small volume or clean samples

Automated Concentration

TheXcelVap®AutomatedEvaporationSystemisamodern,compactbenchtoplaboratoryconcentratorthatprovidesrapid,gentleevaporationofupto54sampleextractsranginginsizeupto200mLeach.Evaporationisaccomplishedbycombiningconsistentheat, controlled sparge gas, and active venting of the solvent vapors.

Horizon XcelVap®

• Automatedpressureprofilingforoptimumspeedwith the most reproducible recoveries • Nozzlescanbeindividuallychangedbytheuser, simplifying maintenance and reducing operating costs• Interchangeableracksaccommodatepracticallyany glassware on the market• Easywaterbathmanagementwithwaterlevelsensor and front draining• Smallfootprint,portraitorientationandexhaustventing help to avoid the need for placement in a fume hood

Visitwww.chromspec.com/evaporation for more information.

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QuEChERS

QuEChERSa Quick,Easy,Cheap,Effective,Rugged,andSafe clean-up method for pesticides and pharmaceuticalsinfoodproducts,biologicalsamplesandsimilaranalytesandmatrices

QuEChERS are easy to use!PreparesamplesforLCorGCanalysisin3simplesteps:

Blend• Homogenizethesample.Addwaterifrequiredtogiveasmoothie-likeconsistencyExtract and Dry• Transfertoacentrifugetube,addacetonitrileandinternalstandard,thenshake vigorously for 1 minute• Addbufferingsaltsandshakeagain.Thesaltstriggeraphaseseparation between the water and acetonitrile extract. Centrifuge for 5 minutes to complete the separation of phasesClean Up• Transferacetonitrileextract(supernatant)toa2nd centrifuge tube, this one containingdSPEmaterial• Shake,centrifuge,andtransfersupernatanttoanautosamplervial,foranalysisby GCorHPLC• Note:Non-targetorganicsaretrappedwiththespentdSPEmaterial(whichwill bediscarded)

$Pre-packed products — save valuable time for increased lab throughput

UCT QuEChERS

• AnextensiveselectionofQuEChERSextractionsaltspre-packedin polypropylenecentrifugetubesorMylarpouches• Customproductsareavailable


Weofferbuffersaltpackagesdesignedtostabiliseacidorbasesensitiveanalytes,anddSPEsorbentpackagesto clean up extracts with different levels of fats, sugars or pigments. Contact our Technical Team for advice on matching kits to your samples.

Restek QuEChERS

$Cutcosts,storagespaceandlabwastebyeliminatingone-timeusePP tubes from your method

Thesesturdy,easy-to-cleanFEPtubeslastindefinitelyundernormalusageconditions.

QuEChERS Optimized Centrifuge• Rugged,pushbuttondesign,atagreatprice• Meetsorexceedsrequirementsoforiginalunbuffered,AOAC, andEuropeanQuEChERSmethodology

Reusable QuEChERS Centrifuge Tubes

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UCT ChloroFiltr®

a Selectively Remove Chlorophyll from Plant Extracts

and Keep Planar Pesticides Intact StandardQuEChERSproducts useGraphitizedCarbonBlack (GCB) to remove chlorophyllfromsamples;althoughGCBiseffective, italsoremovesplanar(polararomatic)pesticides.Low recoveries for these analytes reduce analytical sensitivity and reproducibility. High polarity solventscanbeusedtoremovetheplanarpesticidesfromGCBbutcauseanincreaseinback-groundinterferences(andanextrastep).UCTusesChloroFiltr®inplaceofGCB.

ChloroFiltr® has been tested against hundreds of pesticides and herbicides and has been showntoreducechlorophyllconcentrationbygreaterthan82%withoutlossofplanaranalytes.

NomethodmodificationisnecessarywhensubstitutingChloroFiltr® forstandardGCB-basedmaterials.

ChloroFiltr® is available in a variety of formats to clean between 1 and 12 mL of supernatant.

QuEChERS

Crude SpinachExtract

dSPEcleanupwithChloroFiltr®

dSPEcleanupwithGCB

ChloroFiltr®hasremovedasmuchchlorophyllasGCBandpesticide recoveries are higher.

Planar Pesticides

ChloroFiltr®outperformsGCBforrecoveryandreproducibility

Non-planar Pesticides

ChloroFiltr®providesequivalentperformancetoGCB

Meanrecoveryerrorbarsshow±3 s(95%)confidenceintervalN=4

UCT SpinFiltr™ a

SpinFiltr™ makes dSPE even easier

a 0.22µmfilterensurescompleteseparationofsorbentfromsampleaftercentrifugation



SpinFiltr™stepsarethesameasanydSPE:1. Add sample to sorbent in upper chamber2.Vortex/Shake3.Spin–liquidflowthroughmembrane

Sorbent, drying salt and unwanted matrix stay in the top chamber while puri-fiedextract is filteredandcollected in thebottomportionof the tube.Thechamberisdiscardedandanalystsareleftwithonlypurifiedextractthatisready for analysis.

InconventionaldSPE,theliquidsampledirectlyoverlaysa“pellet”ofsorbentafter spin down. Abrupt handling can easily re-suspend the sorbent and con-taminate samples.

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COLUMNS FOR PHASE SEPARATION

Macherey-Nagel CHROMABOND® PTS / PTL Filtersa

The Ideal Tool for Breaking Emulsions

IfyouareworkingwithLLE,PTS/PLTfiltersprovideautomaticseparationof a two-phase mixture without a separation funnel.

• Two-phasemixturesarecompletelyappliedtothecolumn• Emulsionsareeliminatedasthedenserphasepassesthroughthe membrane, but the lighter phase is trapped above• Membraneautomaticallystopstheflowwhenthedenserphasehas passed• Usesgravityflow–nopressureorvacuumrequired• Upperphaseremainsinthecolumn,bothphasesareavailablefor further analysis

PTS: Forsolventsthatareheavier than water, e.g., for trichloromethane, dichloromethane.Maxsize150mL.

PTL: Forsolventsthatarelighter than water, e.g., for diethyl ether, hexane.Maxsize70mL.

To process larger samples, or for greater automation of your sample preparation, ask us about DryDisk membranes for organic solvents that are denser than water.


CHROMABOND®PTLinaction:Fromlefttoright,PTLallowstheaqueousphase(lower,red)throughthemembrane,andstopstheorganicphase(upper,colourless).

Contact us for more information.

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SOXHLET EXTRACTION

We offer quality supplies at the competitive prices you need! $Soxhlet extraction is an effective method to use when your analytes have limited solubility and the impurity in your sample is insoluble in the desired solvent.

•DisposableThimbles

• 18to80mmIDand37to250mmheight

• CelluloseThimbles-recommendedfor - Standard extraction methods including fats in food, vitamin A and carotene, lacquerandbinderinpaints,qualitymanagementofcomponentsusedin pharmaceutical formulations, organic pollutants in tissues or soils.

• GlassFiberThimbles-recommendedfor -Samplingdustparticlesandaerosolsfromgaseousstreamsupto500°C -Extractionsrequiringsolventstooaggressiveforthecellulosethimbles

• QuartzFiberThimbles-recommendedfor -Emissionstestinginhigh-temperatureenvironmentsupto900°C -Testingacidicgasesnotcompatiblewithmicro-glassfiberthimbles

•ReusableGlassThimbles

• 28to45mmOD,85or125mmheight,and6-160µmporosity •Costeffectiveonlyifcleaningthimblebetweenusesiseffectiveandnottimeconsuming

•Condensers

•Extractors

•Roundbottomflasks

Visitwww.chromspec.com/soxhlet for more information.

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$Reduce Solvent UseMicroSoxhletextractionconsumeslessorganicsolvent.Whenlimitsofdetectionaren’tcrucialorsamplesizeislimited,scaledowntothe10 x 50mm thimbles and save money.

[email protected]

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PURGE & TRAP / THERMAL DESORPTION

Economical Air and Water Volatiles Analysis$CDS 7000E Purge and Trap ConcentratorThe CDS 7000 was acknowledged as a workhorse in the industry for years, now the7000Edeliversthesamecombinationofqualitiesthatmadethe7000suchapopular choice, but in a smaller and more cost effective package.

• Proven,reliableperformance• Easyoperation• Bestvalue/performanceavailable• Autosampleroptionsincludewateronlyorsoil/water

• CDS7300Purge&TrapAutosampleraWater only• CDS7400Purge&TrapAutosampleraWater / Soil / Dynamic Headspace• CDS7500ThermalDesorptionAutosampleraSorbent Tubes for Air Sampling

With this modular platform, you can easily upgrade from the 7300 water-only autosampler to the 7400 or 7500 with a simple swap of towers. Changing from one mode to another can be accomplished in a matter of minutes!

• 72positionswithremovablesampletraysfor40mLVOAvialsorTDtubes• Switchbetweenwater,soilanddynamicheadspacemodesinseconds• Switchingtothermaldesorptiontakesonlyminutes• ConnectstoexistingCDS7000Esystemsaswellasotherconcentratorsand/or desorbers on the market• Performingmultiplemethodsononesystemsavessignificantlyoverthepurchase of multiple systems• Competitivelypriced

CDS 7300 / 7400 / 7500 Series Autosamplersa

Withmodulartowers,itislikehaving3systemsin1!

CDS7300(Wateronly) CDS7400(Water&Soil) CDS7500(TDTubes)

Contact our Instrumentation Team for more information.

Visitwww.chromspec.com/camsco

for information on Camsco Thermal Desorption Tubes.

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ALL-IN-ONE GC AUTOSAMPLERS

HTA HT2800T Autosamplera Static Headspacea SPMEa Liquid Injection

} All-in-one Unit

• Lowestcostofownershipintheindustry

• SuperiorthermalstabilityforSPMEandheadspacemodes

• Touchscreencontrolforexceptionaleaseofuse

• 5+5flexibility:5minutestoswitchbetweenmodes, 5minutestoswitchbetweenGC’s

• WorksonallGCsystemsandallowsfordualinjector configurationsonmostplatforms

• Mountingdesignallowsforinjectormaintenancewithoutmoving the autosampler

• OptionalCFR21Part11compliantsoftware

Smart Technologies for the best user experience

TheHT2800Tfeaturesauniqueportfolioofpatented,proprietaryorlicensedtechnologies:

• Systemintegrityandvialleakagecheckforheadspaceanalysis

• SyringeID:aproprietarytechnologybasedonRFIDtagtoprevent mismatch errors

• Six-positionoventhatallowstheoptimizationofpreparationtimes forheadspaceandSPME

Contact our Instrumentation Team for more information.

• TurnkeySystems • Installation • Customization • MaintenanceandRepairs • Automation • ConsultationandTraining • ProcessIntegration

We offer a solutions-based approach for chromatographyand sample preparation instruments

Contact us for a

Our professional in-house Instrumentation Specialists are available to provide you with a full rangeofservices, includingnewproductinstallation,on-siteserviceandtraining,toll-freetelephone support...and much more.

[email protected]

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SYRINGE FILTERS

CHROMSPEC™…The Name for Affordable Quality

Visitwww.chromspec.com/UV for more information.

Yourbestoptionforqualitysyringefiltersatlowerprices! $


• Solventresistanthousing• MadewithNorthAmericanmembranes• Sterileornon-sterileoptions• GMFpre-filteroption• Poresizesof0.45µmand0.22µmforHPLCandUHPLCapplications• 4mm,13mm,25mmand30mmdiameters• Availablemembranesinclude:GlassFibre,MixedCelluloseEsters, Nylon,PES,Polypropylene,PTFE,PVDFandRegeneratedCellulose

NON STERILE• Greatperformanceforhighthroughputlabs• IdealforHPLC-UVandGC-FIDapplications

STERILE• ETOSterilizedandindividuallysealedtomaintainsterility• Idealforsterilefiltrationandclarification

CHROMSPEC™ UV Syringe Filters

Size Selection

Syringe Filter Size Sample Volume

4mm 2mL 13mm 6mL 25mm 70mL 30mm 90mL

Nylon• Hydrophilic,goodsolventresistanceandmediumprotein binding• Filtrationofallaqueoussamplesandmostorganicsolvents• Notrecommendedforacids

PTFE• Highestsolventresistanceandhighproteinbinding• Filtrationofnon-aqueousorsolventbasedsamples• Recommendedforstrongacidsandbases

PVDF• Highlyresistanttomostsolventsandlowproteinbinding• Generalfiltrationofbiologicalsamples• Filtrationofallaqueousandmostsolventbasedsamples• Filtrationofproteinsandtissuecultures

Mixed Cellulose Esters (MCE)• Hydrophilicandverylowproteinbinding• Idealforaqueousbasedsamples,tissuecultureand sensitive biological samples• Lowchemicalresistance

Choosing the right CHROMSPEC™ UV Syringe FilterPES• Hydrophilicandlowproteinbinding• Idealforaqueousbasedsamples• Generalfiltrationofbiologicalsamples

Polypropylene• Hydrophobic• Highsolventresistance• Lowproteinbinding• Generalfiltrationofbiologicalsamples• Filtrationofallaqueousandmostsolventbasedsamples

Regenerated Cellulose• Hydrophilic• Resistanttomostsolventsandaqueoussolutions (pHrange3-12)

Pre-Filters• Recommendedforremovingparticlesinsuspension• Helpspreventcloggingofthesyringefiltermembrane

Sterile• Applicationsinclude:Cellculturemediaprep,mycoplasma removal,sterilefiltration,includingDMSO

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SYRINGE FILTERS AND FILTER VIALS

Thomson SINGLE StEP Filter Vials

Reducewasteandimprovespeedandefficiencywhenfilteringsamples

Whatman GD/X™ Syringe Filtersa

For samples with high solids content

WhatmanGD/X™syringefilterswithintegratedlayeredpre-filtersaredesignedforexceptionalloadingcapacitywithhighflowratesfor thick, viscous samples.

• Integratedthree-stageglassfibrepre-filter(10µmto0.7µm)removesmoresolidswithoutclogging• Clean,inertandruggedpolypropylenehousing• Poresizesof0.2µm,0.45µmand5µm• 13mmor25mmdiameters• Availablemembranesinclude:Nylon,PES,Polypropylene,PTFE,PVD,RegeneratedCelluloseandCelluloseAcetate

GD/X™filtersprocessthreetoseventimesmoresamplevolumethanfilterswithoutapre-filter.

$• Easytouse:simplyaddyourunfilteredsolutiontothevialbase, squeezethefilterplungerintothebase,andyourvialisready for the autosampler. • Incorporatesvials,caps,syringes,andfiltersintooneunit• Saferthansyringefilters - Vialdesignlimitspressureonmembrane–lessriskofbursting - Fullycontainedsampleeliminatesdangerousaerosolseven ifafilterbursts• AvailableinNylon,PES,PTFEandPVDFmembranematerials

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Isyouranalytenon-volatile,won’tpassthroughaGC,andhardtodetectusingHPLC?

Derivatizationreagentsaredesignedtosimplifychromatographybyincreasingsamplevolatility,allowingforsimpleGC-FIDdetection;orenhanceUV-VisibleabsorptionforroutineHPLCdetection.

Contact our Technical Support Team for assistance in determining the ideal derivatization reagent for your particular analysis.

Chromatographic Specialties Inc. carries reagents from...

General Reagent CategoriesSilylation Reagents• Maskpolargroupswithanalkyl-silylgroup• Improvevolatility• AdditionalcarbonfromalkylgroupsincreaseFIDresponse• ReactwithAlcohols,Phenols,Carboxyls,AminesandAmides

Acylation Reagents• Maskpolargroupswithanacylgroup• Highlyreactive,suitedforanalyteswheresterichindrancemay be a factor• Allacylationreagentsaddcarbons&increaseFIDresponse• Fluorinatedreagentsincreaseelectroncapture,forextremely sensitiveECDmethods• Idealforhighlypolar,multi-functionalcompounds,suchas carbohydrates and amino acids

Alkylation Reagents• Reducepolaritybyreplacingactivehydrogenswithanalkylgroup• Fast,stableandquantitative• IncreasevolatilityandFIDresponse• Modifycompoundssuchascarboxylicacidsandphenols• Commonlyusedtoformesters• Etherandamidesalsopossible

Chiral Analysis of Amphetamines• Regis’TPCreagentisidealforfastandeasyidentificationof amphetamine isomers• 30minutepreptimecreatesdiasteromersforFIDanalysison standardGCcolumns

HPLC Derivatization • Wehaveinstrumentationandsuppliesforpre-andpost-column derivatizationtoaddchromophoresforimprovedHPLCdetection

(formerPierceproducts)

(Post-columnInstrumentstoo)

DERIVATIZATION REAGENTS

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SOLID PHASE MICROEXTRACTION (SPME)SPME,inventedbyDr.JanuszPawliszynattheUniversityofWaterloo,isagreensamplepreparationtechniquethatprovidesrepeat-able results and is easily automated. Applications include food analysis, environmental samples, biologicals, in-vivo analysis, and more... the list continues to grow.

SPMErequiresminimalsamplehandling,saving operators time and laboratory space.

Whichfiberisbestformyapplication?

Choosestationaryphasesandfilmthicknessforyourapplicationbasedonthepropertiesofthecompoundstobeanalyzed.

Target Molecular Analyte Weight* Recommended Fiber Hub Colour

Nonpolar 125-600 7µmpolydimethylsiloxane(PDMS) Green Nonpolar,semivolatile 80-500 30µmpolydimethylsiloxane(PDMS) Golden Volatile 60-275 100µmpolydimethylsiloxane(PDMS) Red Polar,semivolatile 80-300 85µmPolyacrylate(PA) Grey Highlyvolatile 30-225 95µmCarbonwiderange(WR)/PDMS Dark blue

*Thesemolecularweightrangesareareasonableapproximation;however,usersshouldverifysuitabilityfortheirspecificapplication.

Restek PAL SPME Fibers• Reliableperformancethatmeetsorexceedsthecurrent market products• Robustaluminumhubismoredurablethanplastichubs• Colourcodingofhubsfollowsexistingindustrypractice• Fibersare10mmlong,housedina23-gaugeneedle, andhaveastationaryphasebondedtoafusedsilicafiber

HowdoesSPMEwork?

Step1: Readytosample.Fiberiswithdrawnintoneedlefor protection during handling and septum penetration.

Step2: Afterpenetratingsamplevialseptum,fiberisexposedfor absorption by depressing plunger. Absorption can be from headspace(asshown)ordirectfromaliquidsample.

Step3: Fiberiswithdrawnintoneedle,readyforGCinjection.

Step4: Injection.FiberisexposedforthermaldesorptioninGCinlet.

Coming Soon!

Restek SPME Arrow • Optimizedprobegeometryandmaterials• Lifetimeistypically2-3timeslongerthatclassicSPMEfibers• 10timesgreatersensitivitybyproviding15timesmorestationaryphasethanclassic SPMEfibers

Visitwww.chromspec.com/spme for more information.

Colored coded hub(formanual&autosampler)

23 gauge septum piercing needle

Stationary phase coated on fused silica

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SPME Fibre Assembly Detail

SPE Typical Use

SPMEFiberHolder

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Chromatographic Specialties Inc. offers a complete rangeof chromatography solutions including:

•GC Columns, Accessories and Replacement Parts•HPLC Columns, Accessories and Replacement Parts

•Analytical Instrumentation • Chemical Reference Standards•Solid Phase Extraction and Filtration Products

•Glassware and Sample Handling Solutions•Valves and Fittings

CHROMATOGRAPHICSPECIALTIES INC.300 Laurier Blvd., Brockville, ON K6V 5W1Toll Free: 800-267-8103 Fax: [email protected] www.chromspec.com

Background image credit: Can Stock Photo / iulias

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