Modern methods of extraction by Dr. Amit Gangwal

Modern methods of extraction by Dr. Amit Gangwal

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Basics of
Phytochemistry
Dr. Amit Gangwal
(Associate Professor)
SVKM’s Institute of Pharmacy, Dhule
B. Pharm. Vth Semester
Pharmacognosy &
Phytochemistry II
Modern methods of
extraction
(Other than supercritical fluid
extraction)

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commercialinterest,butjusttosharetheeducationalstuff,purelyfrom
academiespointofview.

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Continue….
The flow chart of
medicinal plant
study and
position of
extraction
techniques

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Extractionisessentialforisolationofdifferentchemicalconstituentfrom
crudedrugmaterial.
Extractiondependsonpropertiesofmaterialtobeextracted.
Extractionisdefinedastheprocessofisolationofsolublematerialfroman
insolubleresidue,whichmaybeliquidorsolidbytreatmentwithasolvent
onthebasisofthephysicalnature(solidorliquid)ofcrudedrugtobe
extracted.

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Menstruum:Thesolventcapableofpenetratingthecellwall
ofcrudedrugsanddissolvesalltypesofactiveconstituents
fromitiscalledasMenstruum.Therearetwotypesof
menstruum.
Marc:Theinertinsolublesubstanceleftafterextractionis
calledasMarc.

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Factors affecting extraction process
•Nature of drug
•Nature of extracting solvent
•Solvent temperature
•Ratio of solvent to plant material
•Particle size
•Duration of extraction

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Mechanism of Extraction
•Therefore,solventusedforextractionmustdiffuseintothecelltodissolvethedesired
compoundswhereuponthesolutionmustpassthecellwallintheoppositedirectionand
mixwiththesurroundingliquid
•Anequilibriumisestablishedbetweenthesoluteinsidethecellsandthesolvent
surroundingthefragmentedplanttissues
•Dissolutionofextractivesubstancesoutofdisintegratedcells.
•Dissolutionofextractivesubstancesoutofintactplantcellbydiffusion(requiressteeping
andswelling)
•Penetrationofthesolventintotheplantcellsandswellingofthecells.
•Diffusionofthedissolvedextractivesubstancesoutofthecell.
•Plantconstituentsareusuallycontainedinsidethecells.

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Parameters for Selecting an Appropriate Extraction Method
•Authenticationofplantmaterialshouldbedonebeforeperformingextraction.Anyforeign
mattershouldbecompletelyeliminated.
•Usetherightplantpartand,forqualitycontrolpurposes,recordtheageofplantandthe
time,seasonandplaceofcollection.
•Conditionsusedfordryingtheplantmateriallargelydependonthenatureofitschemical
constituents.Hotorcoldblowingairflowfordryingisgenerallypreferred.Ifacrudedrug
withhighmoisturecontentistobeusedforextraction,suitableweightcorrectionsshould
beincorporated.
•Grindingmethodsshouldbespecifiedandtechniquesthatgenerateheatshouldbeavoided
asmuchaspossible.
•Powderedplantmaterialshouldbepassedthroughsuitablesievestogettherequired
particlesofuniformsize.

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Natureofconstituents:Ifthetherapeuticvalueliesinnon-polarconstituents,a
non-polarsolventmaybeused.Forexample,lupeolistheactiveconstituentof
Crataevanurvalaand,foritsextraction,hexaneisgenerallyused.
Likewise,forplantslikeBacopamonnieriandCentellaasiatica,theactive
constituentsareglycosidesandhenceapolarsolventlikeaqueousmethanolmay
beused.
Iftheconstituentsarethermolabile,extractionmethodslikecoldmaceration,
percolationandCCEarepreferred.

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Forthermostableconstituents,Soxhletextraction(ifnonaqueoussolvents
areused)anddecoction(ifwateristhemenstruum)areuseful.
Suitableprecautionsshouldbetakenwhendealingwithconstituentsthat
degradewhilebeingkeptinorganicsolvents,e.g.flavonoidsand
phenylpropanoids.
Incaseofhotextraction,higherthanrequiredtemperatureshouldbe
avoided.Someglycosidesarelikelytobreakuponcontinuousexposureto
highertemperature.

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Standardizationoftimeofextractionisimportantforexample
insufficienttimemeansincompleteextraction.
Iftheextractiontimeislonger,unwantedconstituentsmayalsobe
extracted.Forexample,ifteaisboiledfortoolong,tanninsare
extractedwhichimpartastringencytothefinalpreparation.

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•Thenumberofextractionsrequiredforcompleteextractionisasimportantasthe
durationofeachextraction.
•Thequalityofwaterormenstruumusedshouldbespecifiedandcontrolled.
•Concentrationanddryingproceduresshouldensurethesafetyandstabilityofthe
activeconstituents.Dryingunderreducedpressure(e.g.usingaRotavapor)iswidely
used.
•Lyophilization,althoughexpensive,isincreasinglyemployed.
•Thedesignandmaterialoffabricationoftheextractorarealsotobetakeninto
consideration.
•Analyticalparametersofthefinalextract,suchasTLCandHPLCfingerprints,should
bedocumentedtomonitorthequalityofdifferentbatchesoftheextracts.

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Types of extraction
•Solidextraction:extractionofsolidfromsolidbyusingappropriatesolvent
•Solventextraction:processinwhichconstituentsthatareextractedbysolid
extractionprocessarepartitionedbetweentwoimmisciblesolvents.

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Steps Involved in the Extraction of Medicinal Plants
In order to extract medicinal ingredients from plant material, the following sequential steps are involved:
1. Size reduction
2. Extraction
3. Filtration
4. Concentration
5. Drying and further purification

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Properties of ideal solvent
1.Be highly selective for the compound to be extracted.
2.Have a high capacity for extraction in terms of coefficient of saturation of the
compound in the medium.
3.Not react with the extracted compound or with other compounds in the plant
material. (inert and non toxic)
4. Must be easily availableand economic.
5.Be harmless to human being and to the environment. (Important)
6.Be completely volatile.

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Infusion
•Freshinfusionsarepreparedbytreatingthecrudedrugforashortperiod
oftimewithcoldorboilingwater.Thedrugisnotboiledwithmenstruum.
•Thesearedilutesolutionsofthereadilysolubleconstituentsofcrude
drug
TypesofInfusion
FreshInfusion:e.g.Infusionoforange
ConcentratedInfusion:Theseusealcoholasmenstruumoritis
usedaspreservative.e.g.ConcentratedinfusionofChirata

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Decoction
•Inthisprocess,thecrudedrugis
boiledinaspecifiedvolumeof
waterforadefinedtime.
•Itisthencooledandstrainedor
filtered.
•Thisprocedureissuitablefor
extractingwater-soluble,heat
stableconstituents.e.g.Tea,
Coffee.

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Digestion
•Thisisaformofmacerationinwhichgentleheatisusedduringthe
processofextraction.
•Itisusedwhenmoderatelyelevatedtemperatureisnotobjectionable.
e.g.extractionofmorphine

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Maceration
•Inthisprocesssolidingredientsare
placedinastopperedcontainerwith
thewholeofthesolventandallowed
tostandforaperiodofatleast3
dayswithfrequentagitation,until
solublematterisdissolved.
•Themixtureisthenstrained(through
sieves/nets),themarcpressedand
thecombinedliquidsclarified
(cleanedbyfiltration)orby
decantation,afterstanding.

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Types of maceration
•Simplemaceration:Processusedformakingtincturesfromorganizeddrugs
E.g.roots,leaves,rhizomes.
•Modifiedmaceration:Processusedformakingtincturesfromunorganized
drugse.g.tinctureoftolu,tinctureofbenzoin.
•Doublemaceration:drugismaceratedtwice.
•Triplemaceration:drugisextractedthreetimesbythemenstrumdividedby
threeparts.

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Process of maceration
•Plantmaterialcrushedorcutsmallormoderatelycoarsepowder,placedina
closedvessels.
•Wholeoftheselectedsolvent(menstruum)isadded.
•Allowedtostandfor3to7days,shakingoccasionally.
•Liquidstrainedoffsolidresidue(marc)pressed,strainedandexpressed
liquidsmixed.
•Clarifiedbysubsidenceorfiltrationevaporationandconcentration

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Percolation
•Itiscontinuousdownward
displacementofthesolventthrough
thebedofcrudedrugmaterialtoget
extract.
•Mostfrequentlyusedtoextract
activeingredientsinthepreparation
oftincturesandfluidextracts.
•Itisthemethodofshortsuccessive
macerationorprocessof
displacement.
•Apercolatoranarrow,cone-shaped
vesselopenatbothendsis
generallyused.

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Steps in percolation
•Sizereduction:Thedrugtobeextractedissubjectedtosuitabledegreeofsizereduction,
usuallyfromcoarsepowdertofinepowder.
•Imbibition:Duringimbibitionthepowdereddrugismoistenedwithasuitableamountof
menstruumandallowedtostandforfourhoursinawellclosedcontainer.
•Packing:Afterimbibitionthemoisteneddrugisevenlypackedintothepercolator.
•Maceration:Afterpackingsufficientmenstruumisaddedtosaturatethematerial.The
percolatorisallowedtostandfor24hourstomaceratethedrug.
•Percolation:Thelowertapisopenedandliquidcollectedthereinisallowedtodripslowly
atacontrolledrateuntil3/4thvolumeofthefinishedproductisobtained.

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Soxhlet Extraction

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Soxhlation
•Materialcoarselypoweredandplacedinsidethethimble.
•Thinlayerofcottontobeplacedatthebottomofthimbleinordertoavoidtheentryof
drugparticlesintosiphontube.
•Toplayerofdrugalsocoveredwithcottoninordertoavoiddisturbancetodrugby
solventaddition
•Aportionoftheapparatustogetherwithsidetube,thimbleandsiphontubeisknown
assoxhletextractor.
•Thisassemblyisattachedtoroundbottomflask.
•Fromtopsolventisaddedslowly.
•Condensorisattachedtothesoxhletassembly.
•Thewholeassemblyissetonheatingmantleandmantleisswitchedon.

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•Oncethesolventbeginstoboil,thesolventvapourtravelstocondenserand
fallsintothethimbledissolvingoutthedesiredcomponentfromdrug.
•Whenthethimbleisalmostfull,itgetsemptiedintotheRBFthroughthe
siphontube.Thecycleisrepeatedseveraltimes.

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Merits and demerits
Merits
•Largeamountofdrugcanbeextractedwithmuchsmallerquantityofsolvent.
•Tremendouseconomyintermsoftime,energy&ultimatelyfinancialinputs.
•Smallscaleusedabatch-process.
•Becomesmoreeconomicalwhenconvertedintocontinuousextraction.
Demerits
•Notfitforalldrugs.
•Notfitforenvironmentvssupercriticalfluidextraction

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Theindustrialprocessingofmedicinalandaromaticplantsstartswiththeextractionoftheactive
componentsusingvarioustechnologies.Thegeneraltechniquesofmedicinalplantextractioninclude,but
notlimitedto:
maceration,
•infusion
•percolation
•digestion
•decoction
•hotcontinuousextraction(Soxhlet)
•aqueous-alcoholicextractionbyfermentation
•counter-currentextraction
•microwave-assistedextraction
•ultrasoundextraction(sonication)
•supercriticalfluidextraction
•phytonicextraction(withhydrofluorocarbonsolvents)

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Foraromaticplants
hydro-distillationtechniques(waterdistillation,steamdistillation,water
steamdistillation),
hydrolyticmacerationfollowedbydistillation,expressionandenfleurage
(coldfatextraction)maybeemployed.
Someofthelatestextractionmethodsforaromaticplantsinclude
headspacetrapping
solidphasemicro-extraction
protoplastextraction
microdistillation
thermomicrodistillation
moleculardistillation

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Microwave-assisted extraction (MAE)
•Microwaveisaformofelectromagneticradiationwithwavelengths
rangingfromabout1meterto1millimetercorrespondingto
frequenciesbetween300MHzand300GHzrespectively.
•Theprefixmicroindicatesthatmicrowavesareshorterwavelengths
comparedtoradiowaves.
•Inordertoavoidinterferenceswithradiocommunications,
domesticandindustrialmicrowavesgenerallyoperateat2.45GHz.
•Owingtotheirelectromagneticnature,microwavespossesselectric
andmagneticfieldswhichareperpendiculartoeachother.
•Theelectricfieldcausesheatingviatwosimultaneousmechanisms,
namely,dipolarrotationandionicconduction.

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•Microwave-assistedextractionoffersarapiddeliveryofenergytoa
totalvolumeofsolventandsolidplantmatrixwithsubsequentheating
ofthesolventandsolidmatrix,efficientlyandhomogeneously.
•Componentsofthesampleabsorbmicrowaveenergyinaccordanceto
theirdielectricconstants.
•Whenplantmaterialisimmersedinsideamicrowavetransparent
solvent,theheatofmicrowaveradiationdirectlyreachestothesolid
withoutbeingabsorbedbythesolvent,resultingininstantaneous
heatingoftheresidualmoistureinthesolid.

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•Heatingcausesthemoisturetoevaporateandcreatesahighvapor
pressurethatbreaksthecellwallofsubstrateandreleasesthe
contentintosolvent.
•Theextractingselectivityandtheabilityofthesolventtointeract
withmicrowavescanbemodulatedbyusingmixturesofsolvents.
•Oneofthemostcommonlyusedmixturesishexane-acetone.

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A a programmable laboratory microwave oven extraction system
(RTP-Plus MARS-S model, CEM Corporate Matthews, NC, USA)

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•MAEtechniquescanbeclassifiedaccordingtothepressurethroughwhich
theyoperate:higherthantheatmosphericpressure(closedMAEsystem)and
lowerthantheatmosphericpressure(openMAEsystem).
•Asregardsclosedsystems,thetemperatureissetovertheboilingpointofthe
solventandthepressureisundercontroltoavoidanexcessivedevelopment.
•Amongtheclosedsystemswecanenumeratehighpressuremicrowave
assistedextraction(HPMAE)whichuseshighpressureandtemperaturein
ordertoenhancethecapacityofthesolventtoincorporatetheenergyfrom
radiationandtoavoidlargeamountofsolventfortheextraction.

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Incaseofthermolabilemolecules,softconditionsareneededandsothechoicewillfall
onanopensystemorthevacuummicrowaveassistedextraction(VMAE)thatallows
thereductionoftheboilingpointofthesolvent.
Forcompoundsthataresusceptibleofoxidationithasbeendevelopedthenitrogen-
protectedmicrowave-assistedextractionoperatingunderpressurizedinertgas.
Whenthebioactivecompoundsaresusceptibleofhydrolysissuchastheessential
oils,solvent-freemicrowave-assistedextraction(SFME)isusedtoavoidthe
loss/degradationoftheseproducts.

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AnotherparametertoconsiderinMAEisthepowerofextraction:an
increasedpowerbooststhetemperaturereducingthesolventviscosity
andleadingtoabetterefficiency,exceptincaseofthermolabile
molecules.

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Applications of microwave-assisted extraction
•MAEcanextractnutraceuticalsproductsfromplantsourcesinafaster
mannerthanconventionalsolid–liquidextractions.
•MAE(80%methanol)coulddramaticallyreducetheextractiontimeof
ginsengsaponinfrom12husingconventionalextractionmethodstoafew
seconds.

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•ExtractionoftaxanesfromTaxusbrevifolia
•AzadiractinrelatedlimonoidsfromAzadirachtaindicaseedkernels
•ExtractionofglycyrrhizicacidfromGlycyrrhiziaglabraroots
•ExtractionofartemisininfromArtemisiaannua
•Ahighermicrowavetemperatureandashortextractiontimearemoreeffectivein
extractinganti-oxidativephenoliccompoundsfromtomato
•Ithasbeenprovenasapotentialalternativetotraditionalmethodsforextraction
ofphenols,suchaschlorogenicacids,fromgreencoffeebeans.

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Advantages of microwave-assisted extraction
•Itreducessolventconsumption.
•Ithasashorteroperationaltime.
•Hasagoodreproducibilityandminimalsamplemanipulationforextractionprocess.
•Microwave-assistedextractiongivesseveraladvantageswithrespecttoclassical
extractiveprocessessuchasSoxhlet.MAEallowsagainoftime,higherqualityand
yields.
•Itisalsocheaperthansupercriticalfluidextraction(SFE)andfasterthanultrasonic-
assistedextraction(UAE).

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Disadvantages of microwave-assisted extraction
•Itrequiresspecializedsetup.
•Anadditionalfiltrationorcentrifugationisnecessarytoremovethesolidresidueduring
MAE.
•Furthermore,theefficiencyofmicrowavescanbeverypoorwheneitherthetarget
compoundsorthesolventsarenon-polar,orwhentheyarevolatile.
•ItismoreexpensivethanUAE.
•LessecofriendlythanSFEduetotheuseoforganicsolvents.
•Notsuitableforthermolabilecompoundsbecausetheirradiationcouldpromotechemical
reactionswiththelossofthedesirableproducts,andnotefficientwhenthetarget
moleculesand/orthesolventofextractionarenon-polarbecausetheydonotabsorb
energyfromthesource.

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Ultrasonication-assisted extraction (UAE)
•Theprocedureinvolvestheuseofultrasoundwaves,
whichhavefrequencieshigherthan20KHz,havegreat
effectsonextractionyieldandkinetics.
•UAEinvolvesultrasoniceffectsofacousticcavitations.
Underultrasonicactionsolidandliquidparticlesare
vibratedandacceleratedand,becauseofthatsolute
quicklydiffusesoutfromsolidphasetosolvent.
•Ultrasoundassistedextractorsareultrasonicbathsor
closedextractorsfittedwithanultrasonichorn
transducer.Themechanicaleffectsofultrasoundinduce
agreaterpenetrationofsolventintocellularmaterials
andimprovemasstransfer.
(meansthespontaneous
formationofbubblesina
liquidbelowitsboilingpoint
resultingfromstrong
dynamicstressing),

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Sonicationistheactofapplyingsoundenergytoagitateparticlesina
sample,forvariouspurposessuchastheextractionofmultiplecompounds
fromplants,microalgaeandseaweeds.
Ultrasonicfrequencies(>20kHz)areusuallyused,leadingtotheprocess
alsobeingknownasultrasonicationorultra-sonication.
Inthelaboratory,itisusuallyappliedusinganultrasonicbathor
anultrasonicprobe,colloquiallyknownasasonicator.

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UAEisbasedontheproductionofultrasoundwavesandtheirtransmissionthroughoutthesolventwitha
resultingcavitation.Whenthecavitationbubblescollapse,thereisagenerationofliquidcirculationcurrentsand
turbulencethatimprovethemasstransferrate.
Thefracturesformedinthecellwallenhanceitspermeabilityandsoabiggeramountofsolventcanenterintothe
planttissuestoextractthebioactivemetabolites.
Inordertoperformanextractionbasedonsonochemistry,thechoiceofsolventbecomesanimportantparameter
becauseitsphysicalpropertieslikepolarity,viscosity,vaporpressureandsurfacetensioninfluencethecavitation
phenomena.
Ethanol,methanolandhexanearewidelyusedinUAE,andsometimeswatercouldbeaddedtoethanol,evenifits
amountmustnotbetoomuchinordertoavoidadecreaseinextractionefficiency,probablyduetothegeneration
ofradicalsfromtheultrasonicdissociationofwater.

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An ultrasound sonicator UP200S manufactured by Dr. Hielscher,
Teltow, Germany

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Otherparameterstobeconsideredarethefrequencyandthepower:oftenthe
formerrangesfrom20to100kHzandthelatterfrom100to800W.
Alsothepowerdissipationisacriticalfactor,becausethegenerationof
physicaleffectsliketurbulenceisdirectlyproportionedtothepowerdissipated
asheat.

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Applications of ultra sonicated extraction
•Usedtoextractnutraceuticalsfromplantssuchasessentialoilsandlipids
dietarysupplements.e.g.oilsfromalmond,apricotandricebran
•Extractionofsaponinfromginseng,theobservedtotalyieldandsaponinyield
increasedby15and30%,respectively.
•Itwasfoundthatricebranoilextractioncanbeefficientlyperformedin30min
underhigh-intensityultrasoundeitherusinghexaneorabasicaqueous
solution.
•Extractionratesofcarvoneandlimonenebyultrasound-assistedextraction
withhexanewere1.3–2timesmorerapidthanthosebytheconventional
extractiondependingontemperature.

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Advantages of ultra sonicated extraction
•Itincreasesextractionyieldandhasfasterkinetics.
•Itreducetheoperatingtemperatureallowingtheextractionofthermolabilecompounds.
•Comparedwithothernovelextractiontechniquessuchasmicrowave-assistedextraction,
theultrasoundapparatusischeaperanditsoperationiseasier.
•UAEislessexpensivethanthetraditionalextractivetechniques;itcangivehighquantities
ofproductswithoutspendingtimeandwithoutusinglargeamountsofsolvent.
•Forabetterperformance,UAEcanalsobeusedincombinationwithothertechniqueslike
supercriticalfluidprocess.

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Disadvantages of ultra sonicated extraction
•Lowerefficiencyascomparedtoothertechniques.
•Althoughtheprocessisusefulinsomecases,likeextractionofrauwolfiaroot,itslarge-
scaleapplicationislimitedduetothehighercosts.
•Thismethodisnotusefulforcommercialpurpose.
•AnotherproblemthatcurrentlylimitstheuseofUAEatlargescalesistheerosionof
transducersandtheircontinuousreplacementtoavoidadecreaseinthetransmitted
energy.
•Forthefuture,thedesignofreactorsbasedonmultipletransducersisneededinorderto
operateatmultiplefrequenciesandimprovetheefficacyofUAE.
•Onedisadvantageoftheprocedureistheoccasionalbutknowndeleteriouseffectof
ultrasoundenergy(morethan20kHz)ontheactiveconstituentsofmedicinalplants
throughformationoffreeradicalsandconsequentlyundesirablechangesinthedrug
molecules.

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Concentrations of main phenolic compounds in nettle extracts obtained by
different methods with1:30 solid to solvent ratio and detected by HPLC (mg/g
dry material)

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•Incounter-currentextraction,wetrawmaterialispulverizedusingtoothed
discdisintegratorstoproducefineslurry.
•Thematerialtobeextractedismovedinonedirection(generallyintheform
offineslurry)withinacylindricalextractorwhereitcomesincontactwith
extractionsolvent.
•Thefurtherthestartingmaterialmoves,themoreconcentratedtheextract
becomes.
•Finally,sufficientlyconcentratedextractcomesoutatoneendofthe
extractorwhilethemarc(practicallyfreeofvisiblesolvent)fallsoutfromthe
otherend.
42
Counter-Current Extraction

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Advantages
•Aunitquantityoftheplantmaterialcanbeextractedwithmuchsmaller
volumeofsolventascomparedtoothermethodslikemaceration,decoction,
andpercolation.
•Itiscommonlydoneatroomtemperature,whichsparesthethermolabile
constituentsfromexposuretoheatwhichisemployedinmostother
techniques.
•Asthepulverizationofthedrugisdoneunderwetconditions,theheat
generatedduringcomminutionisneutralizedbywater.Thisagainsparesthe
thermolabileconstituentsfromexposuretoheat.
•Theextractionprocedurehasbeenratedtobemoreefficientandeffective
thanContinuoushotextraction.

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Itisacontinuousprocessofextractionwhichfacilitatesextractionof
activeconstituentsfromtwoimmisciblesolvents.Allheatstable
Phytoconstituentscaneasilyextractedbythismethod.
Itrequiresmoresolventthantheothermodeofextractiontechniques.
Disadvantages

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Theapplicationsofcounter-currentextractioncoveredmanyfieldsofplant
chemistry,includingalkaloids,aminoacids,antibiotics,antitumour
compounds,phenolsincludinganthraquinonederivatives,cardiac
glycosides,essentialoils,fattyacids,plantauxins,prostaglandins,
steroidsandvitamins.
Othermorerecentdevelopmentsinvolvingthecounter-currentPrinciple
arehigh-speedcounter-currentchromatography(planetcoilcentrifugal
CCC),dropletcounter-currentchromatography(DCCC)andcentrifugal
dropletCCC.

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Anewsolventbasedonhydrofluorocarbon-134aandanewtechnologyto
optimizeitsremarkablepropertiesintheextractionofplantmaterialsoffer
significantenvironmentaladvantagesandhealthandsafetybenefitsover
traditionalprocessesfortheproductionofhighqualitynaturalfragrantoils,
flavorsandbiologicalextracts.
AdvancedPhytonicsLimited(Manchester,UK)hasdevelopedthispatented
technologytermed“phytonicsprocess”.Theproductsmostlyextractedbythis
processarefragrantcomponentsofessentialoilsandbiologicalor
phytopharmacologicalextractswhichcanbeuseddirectlywithoutfurther
physicalorchemicaltreatment.
Phytonics Process

64. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
•Unlikeotherprocessesthatemployhightemperatures,thephytonicsprocessiscoolandgentle
anditsproductsareneverdamagedbyexposuretotemperaturesinexcessofambient.
•Novacuumstrippingisneededwhich,inotherprocesses,leadstothelossofpreciousvolatiles.
•TheprocessiscarriedoutentirelyatneutralpHand,intheabsenceofoxygen,theproducts
neversufferacidhydrolysisdamageoroxidation.
•Thetechniqueishighlyselective,offeringachoiceofoperatingconditionsandhenceachoiceof
endproducts.
•Itislessthreateningtotheenvironment.
•Itrequiresaminimumamountofelectricalenergy.
•Itreleasesnoharmfulemissionsintotheatmosphereandtheresultantwasteproducts(spent
biomass)areinnocuousandposenoeffluentdisposalproblems.
•Thesolventsusedinthetechniquearenotflammable,toxicorozonedepleting.
•Thesolventsarecompletelyrecycledwithinthesystem.
Advantages

65. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Thephytonicsprocesscanbeusedforextractioninbiotechnology(e.gfortheproductionof
antibiotics),intheherbaldrugindustry,inthefood,essentialoilandflavorindustries,andinthe
productionofotherpharmacologicallyactiveproducts.
Inparticular,itisusedintheproductionoftopqualitypharmaceutical-gradeextracts,
pharmacologicallyactiveintermediates,antibioticextractsandphytopharmaceuticals.
However,thefactthatitisusedinalltheseareasinnowaypreventsitsuseinotherareas.The
techniqueisbeingusedintheextractionofhigh-qualityessentialoils,oleoresins,naturalfoodcolors,
flavorsandaromaticoilsfromallmannerofplantmaterials.
Thetechniqueisalsousedinrefiningcrudeproductsobtainedfromotherextractionprocesses.It
providesextractionwithoutwaxesorothercontaminants.Ithelpsremovemanybiocidesfrom
contaminatedbiomass.
Applications

66. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Ionic liquid Mediated Extraction (Ils)
Theuseofionicliquidforanalyticalpurposeshasbeendevelopedinmodern
timeswithadvantagesintermsofqualityandefficacyofextraction.
Inparticular,anionicliquidconsistsofaliquidorganicsaltthatselectively
interactswithspecificpolarandnon-polarcompoundsthankstoion-exchanges,
π-stackinginteractions,hydrophobicinteractionsorhydrogenbonds,improving
theselectivityoftheextractivemethod.

67. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Forexample,theinteractionof1-butyl-3-methylimidazoliumhexafluorophosphate
([BMIM][PF6])withhydrophilicaminoacidsenhancestheextractionefficiencywith
respecttoatraditionalorganicsolventextraction.
BeingILsappliedinseveralextractiveprocessessuchasMAEandUAE,they
shouldbestableenoughtoresisttothehightemperaturesthroughwhichthe
techniqueworks.
Aboutthismatter,tetraalkylammoniumcationsandimidazoliumionslike
tetrafluoroborate[BF4]−,bis(trifluoromethylsulfonyl)imide[NTf2]−,
trifluoromethanesulfonate[CF3SO3]−,andhexafluorophosphate[PF6]−,possessa
greatthermalstability;moreover,theorganicanionshaveshowntobemorestable
thantheinorganiconeswhenoperatingatelevatedtemperatures.

68. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
In conclusion, extraction based on ILs represents a good choice to
recover in high yields organic and inorganic and metal ions as bioactive
components of plants and herbs.
ILsareliquidmoltensaltsattemperaturesbelow100°Candaretypicallycomposedoflarge
andunsymmetricalorganiccationsandorganicorinorganicanions.Beyondtheexcellent
chemical,thermal,andelectrochemicalstability,noflammability,andnegligiblevolatility
displayedbymostaproticILs,ILsarealsorecurrentlyrecognizedbytheirexcellentsolvation
abilityforawiderangeofcompoundsandmaterials,fromsyntheticallyproducedtonatural
extractedones,andasgoodstabilizingmediaforproteins,enzymes,nucleicacids,among
others.

69. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Pressurized liquid/fluid extraction (PLE)
Pressurizedliquidextraction(PLEorPFEincaseofageneralfluid)isanoveland
eco-friendlyapproachfortherecoveryofbioactivesfromplants.
Thismethodoftenrequireswaterasthesolventandsoitcankeepawayfromthe
environmentalandhealthrisksduetotheuseoforganicsolvents.
Operatingathightemperature(till200°C)andpressure(from35to200bar),PLE
improvesthequalityoftheextractionthatcanbecarriedoutinadynamicmode
inwhichthesolventisincessantlypumpedthroughthevessel,orinastaticmode
inwhichtherearemorecycleswithacontinuousreplacementofthesolvent.

70. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals

71. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Atelevatedtemperaturesthereisareductionoftheviscosityofthesolventthatcanbetter
penetratethematrixextractingtheanalytesofinterest,evenifthisapproachcannotbe
usedforthethermallyunstablecompoundsanditcouldleadtoaco-extractionofother
compoundsbecauseofthedecreasedselectivityofextractionathighertemperatures.
Theelevatedpressurepermitsmaintainingthesolventintheliquidphaseandthe
disruptionofplantcellswallexertingpressureonthematrix.Inplaceoforganicsolvents,it
ispossibletouseadditiveslikenon-ionicsurfactants,antioxidantslikeascorbicacid,CO2
todropaqueouspHordryingagents.
Furthermore,PLEapparatusprotectslightsensitiveandoxygensensitiveproductsfrom
degradation,anditcouldbehyphenatedwithothermodernextractivetechniqueslikeUAE
toimproveitsefficacy.

72. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Enzyme-assisted extraction
Analternativeapproachtoclassicalsolventextractiontechniquesistheenzyme-assisted
extraction.Thismethodisinnovativeandconvenientthankstothefactthattheenzymes
catalyzereactionsinaspecificwaywithoutoperatingunderstrongconditionsthatcould
leadtothedegradationofthedesiredproducts.
Inaddition,proteinslikecellulases,hemicellulasesandpectinasesdisruptcellwallwiththe
hydrolysisofitscomponentsleadingtoamajorpermeabilityandallowinganeasierrelease
ofthemetabolitesfromplants.
Theapplicationofenzymessuchaslipases,proteases,phospholipases,permitstoreduce
theuseofthesolventfortheextraction.Foroilextractionfromplants,cellulase,α-amylase
andpectinasearethemostusedenzymes.

73. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Theseproteinscanbeobtainedfromfungi,bacteria,animals,andvegetablesor
fromgeneticengineeringmethodsand,thankstotheirselectivecatalysis,they
canbeusedtorecoveraspecificbioactivecompoundinhighyieldsandina
“green”approach,withoutwastingtoomuchenergy.
Nevertheless,therearesomelimitationsduetothecostoftheenzymatic
approach,theincompletedisruptionofthecellwallandthecomplicated
applicationinacommercialscalebecauseofthedifferentbehaviorofthe
enzymesaccordingtotheenvironmentalcircumstancessuchastheamountof
oxygen,thevarietyofnutrientsandtheoperatingtemperature.

74. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals

75. Vision: To Pursue Excellence in Pharmaceutical Education & Research to Develop Competent Professionals
Thanks