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Decoction and Hot Continuous Extraction Technique

Decoction and Hot Continuous Extraction Technique

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Published by: Nguyen Bich Anh on Sep 07, 2010
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11/13/2011

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DECOCTION AND HOT CONTINUOUS EXTRACTION TECHNIQUES

Sudeep Tandon Scientist Chemical Engineering Division CIMAP, Lucknow

INTRODUCTION
Decoction is a water-based preparation to extract active compounds of herbs, made by boiling the plant parts for some period. Used to primarily extract the mineral salts and bitter principles of plants, rather than vitamins and volatile ingredients It is a liquid preparation made by boiling the herbs with water, differing from infusions that the latter are not actively boiled Decoctions are usually the method of choice when working with tougher and more fibrous plants, barks and roots (and which have water soluble chemicals).

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• Instead of just steeping it in hot water, the plant material is boiled for a longer period of time to soften the harder woody material and release its active constituents • The plant materials are generally into broken into small pieces or grounded into a powder—the smaller they are, the more easily they will be absorbed into the water • More heat is needed in making decoctions than infusions, since mostly the parts of the herb that are used in decoctions—the bark and roots—are very dense in nature. • Unfortunately, the high heat does tend to destroy some of the herb's volatile oils.

Methods of preparing decoctions

Different methods have been described in literature for preparation of decoctions…

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Place the lid on the pot and reduce the heat to medium or medium-low so that the mixture stays at a good simmer. Measure the amount of herb needed into the pot and add the proper amount of cold water depending on how many cups of the decoction you wish to prepare. If using powdered herb. strain the mixture through a strainer When straining. select a ceramic pot (Material can vary) with a snug fitting lid.… To prepare a decoction.4 times water If drug is moderately hard – 8 times water If drug is very hard – 16 times water • Then boiled on low flame till reduced to 1/4th in case of soft drugs 1/8th in case of moderately or very hard drugs • Cooled. strained and filtrate collected in clean vessels IN ANOTHER METHOD DESCRIBED ELSEWHERE ……. make sure to press on the cut herb pieces in the strainer to get as much liquid/decoction out of the herb pieces as possible. allow the powder to settle to the bottom of the pot and then pour off the decoction from the top 3 . Turn on the heat to medium high and bring to a boil.METHOD FOR PREPARING DECOCTIONS IN TSM / AYURVEDA • Traditionally known as ‘KWATHA’ • Methodology : The Drug in form of ‘Yavakuta’ (small pieces taken in earthen pots or tinned cooper vessel with clay on outside If drug is soft. Simmer it covered for certain fixed time or till volume of water reduces to fixed ratios Remove from heat and cool slightly. If using cut herbs.

• The first involves boiling the mixture longer.. soften. strong decoctions are prepared in two general ways. = 50 gm • Water. when smaller woody pieces are used yet a stronger remedy is wanted. then it is allowed to sit/soak overnight before straining out the herb. • Alternatively. the decoction is prepared as above (boiling 20 minutes).. and extract the larger pieces. This is usually indicated when working with larger woody pieces of bark. Longer boiling time. is sometimes necessary to break down. • Only Recently prepared decoctions should be dispensed • Decoctions should be stored under refrigerated conditions • The drug concentration of a decoction should be well specified for the plant material or should be prescribed by a physician If drug concentration is not specified then following general formula of USP XII can be used • The Drug.. coarsely comminuted ……………. cover it and boil for about 15 min • Allow to cool to 40oC • Strain and use as such or dilute again to 1000 ml 4 . sufficient quantity……………….STRONG DECOCTIONS • Depending on the type of plant material used.to make 1000 ml Method • Place the drug in a suitable vessel provide with a cover • Pour upon t 100 ml of cold water. up to 2 hours or more.

glycosides etc Extracts which contain bio active constituents for further downstream processing and isolation of the pure phytomolecules Aromatic plants mostly florals like rose. jasmine. saponins. tuberose for preparation of concretes and absolutes Spices or spice plants for preparation of the oleoresins / resenoids 5 .Extraction with Volatile solvents Mainly applied for Medicinal plants /herbs for preparation of standardized extracts / total crude extracts like alkaloids.

• It is customary to calculate the number of ideal (equilibrium) stages required for a given leaching task 6 .e. more often it is particulate. the equilibrium line will be straight line through the origin with a slope of unity. • The rate of mass (Δ m) transfer in the time dt is a function of surface contact between the phases (S). ΔM = SD (Cs – C) Concept of Equilibrium s • The practical interpretation of leaching equilibrium is the state in which the overflow and underflow liquids are of the same composition. The stream of solids being leached and the accompanying liquid is known as the underflow The solid content of the stream is sometimes called marc. The stream of liquid containing the leached solute is the overflow PRINCIPLE OF SOLVENT EXTRACTION • When solvent penetrates into plant material it is necessary. of the coefficient diffusion of the solute in the solution (D) and of the concentration of the solute in the liquid (C) to the time t and in the liquid film around the solid that we are extracting (Cs) as well as the thickness of the liquid film around the solid matrix (S). The separation usually involves selective dissolution. i. Lixiviation is also used less frequently as a synonym for leaching The insoluble solid may be massive and porous. and the particles may be openly porous. to verify the diffusion process. cellular with selectively permeable cell walls.Solvent Extraction of herbs fall in category of solid liquid extraction and is also referred as the leaching process Leaching is the process of removing a solute from a solid by the use of a liquid solvent. with or without diffusion. the mass transfer of the product from the solid phase to the liquid. on a y-x diagram. or surface-activated.

2. Contact of liquid solvent with the solid to effect transfer of solute from the solid to the solvent. Two other auxiliary operation are involved namely : a) Preparation of the solid for extraction and b) Recovery of solute form the solvent.TWO STEPS ARE ALWAYS INVOLVED IN SOLID LIQUID EXTRACTION 1. Separation of resulting solution from the residual solid. usually by evaporation or distillation of solvent from the solute MECHANISMS OF EXTRACTION Single Stage Extraction : OVERFLOW SOLUTION FRESH SOLVENT EXTRACTION STAGE SOLID UNDERFLOW SOLID FEED Multistage Co current Extraction Fresh Solvent Fresh Solvent Extraction Stage 1 Solid Feed Overflow Solution Overflow Solution Overflow Solution Extraction Stage 2 Fresh Solvent Extraction Stage n Solid Under flow Multistage Counter current Extraction Fresh Solvent Extraction Stage1 Solid Under flow Extraction Stage 2 Extraction Stage n Solid Feed Overflow Solution 7 .

therefore the degree of comminution need not be great. The cells are. Many pharmaceutical products recovered from plant roots. whereas hard and woody substances will require a greater reduction in size. and these does much toward rupturing the cell walls and releasing the solute for direct action by the solvent. 8 . is it thick or thin ? If the drug is leaves or petals then it will be easily penetrated by the solvent. stems and leaves.PROCESS PARAMETERS EFFECTING SOLID LIQUID / SOLVENT EXTRACTION • MATRIX CHARACTERISTICS • CHOICE OF SOLVENT • METHOD OF CONTACTING • TEMPERATURE OF EXTRACTION • NUMBER OF WASHES • CONDITIONS FOR EXTRACTION-AGITATION MATRIX CHARACTERSTICS Solvent extraction strongly depends on matrix characteristics and particle size as the internal diffusion may be limiting step during extraction. and constituents are then more rapidly contacted by the solvent. of course smaller than this.g. is it hard or soft ?. but they are largely ruptured by the flaking process. the plant material is frequently dried before treatment. The degree of comminution required will also depend on the composition of the crude drug e.

β = Selectivity : Insolubility / Miscibility of Solvent Low boiling point and high volatility for better Recoverability Polarity Solvent should be non toxic Non flammable & low cost Non Denaturing nature Chemically non-reactive towards the product being extracted ECOFREINDLY 9 .e.CHOICE OF SOLVENT : Wt fraction of solute in Residue Wt fraction of solute in Extract Selectivity must exceed unity (i. > 1) the more so better.

consideration. solvent-vapor pressure. Elevated temperature. Use of high temperature during extraction is avoided when the active constituents are thermo labile or volatile and to reduce the level of unwanted constituents.77 69 78 34.∞ = completely miscible TLV : Threshhold Limit Values TEMPERATURE Higher temperatures results in greater solubility of solvents and and therefore are sometimes desirable to realize higher solute concentration in the extract. in case of some natural materials may result in excessive extraction of undesirable material.m . m = miscible.t = < 0.5 80. 10 .7 61 76.01%.7 91 82.SOME COMMON SOLVENTS USED FOR EXTRACTION OF MAP’S Solvent Acetone Aceric Acid Ethyl Acetate Benzene Buthan-2-one Cyclohexane Dichloromethane Chloroform Carbon tetrachloride Hexane Ethanol Ethyl ether Petrol ether Propantriole Methanol 1-propanol 2-propanol tolune BP (OC) 56 116-117 77 80 79.7 39.p. and sensitivity of product.2 ∞ ∞ M M? 0. solute diffusivity.8 T ∞ 1.06 TLVb 1000 10 400 25 2200 300 2200 50 10 1000 400 500 200# 400 400 100# b . The temperature of the extraction should be chosen for the best balance of solubility.3 8 0.4 110.6 Miscibility with H2 O ∞ ∞ 80 T 19 T 1. * = with decomposition. solventsolvent selectivity. Higher temperature operation may also not be permissible because of solvent losses and for safety consideration.p.6 30-50 290* 64.

11 . EACH CAN BE EITHER BATCH AND CONTINUOUS UNITS. Solvent may be contacted with a fixed bed of solids in three different ways: 1) Spray Percolation 2) Full immersion 3) Intermediate drainage. the solid particle are stationary. While dispersed contact involve motion of solid particles relative to each other and also relative to liquid. Solid – Liquid Extraction: Equipments Can be divided into two main classes : 1) Those in which the leaching is accomplished by percolation (Passing the solvent through a bed of static particulate material) 2) Those in which particulate solid are dispersed into a liquid and subsequently separated from it.METHOD OF SOLID LIQUID CONTACTING In fixed bed contacting.

They are sprayed with solvent until their solute content is reduced to an economic minimum and are then excavated. The technique is sometimes referred to as total extraction. CONTINUOUS PERCOLATORS Coarse solids are also leached by percolation in moving-bed equipment. The solids to be leached are dumped into the tank to a uniform depth. it is a large circular or rectangular tank with a false bottom. including single-deck and multideck rake classifiers. Countercurrent flow of the solvent through a series of tanks is common. bucket-elevator contactors. and horizontal-belt conveyors. It is referred to as soft extraction technique. both of which may cause damage to the constituent of the whole herb. BATCH PERCOLATORS The batch tank is not unlike a big nutsche filter.PERCOLATION Percolation is generally carried out in batch tanks and in continuous or dump extractors (usually on smaller scale). 12 . COLD PERCOLATION : This method allows processing of the herbs into a liquid extract without utilizing heat or concentration. HOT PERCOLATION : In this method the bio-mass is added to the container containing the solvent and the mixture is heated under reflux. with fresh solvent entering the tank containing most nearly exhausted material.

contact fashion. on the other hand . Agitation • If a solid in the form large lumps is to be leached. can be avoided by stirring the liquid and solid in leaching vessel.Leach more slowly and possibly less thoroughly but on draining may retain relatively little solution. • Agitation operates in stage wise or in continuous. with its consequents slow and incomplete leaching. 13 . probably because the large amount of static liquid holdup makes important amounts of solute unavailable.Vessels with Agitation • Channeling of the solvent in percolation of fixed bed. a decision must frequently be made whether to crush it coarse lumps and leach by percolation or whether to grind it fine and leach by agitation • Fine grinding is more costly but provides more rapid and possibly more thorough leaching. whereas continuous-contact equipment may provide the equivalent of many stages in a single device. and thus provide a more concentrated final solution.. require less washing. • The agitation vessel is generally used for coarse solids • This device is operated in batch wise fashion and provides a single leaching stage. • Stage wise equipment is sometimes assembled in multiple units to produce multistage effects. Percolation Vs. • Leaching is generally more efficient in a thoroughly agitated vessel then by percolation. • Coarsely ground particles.

Disadvantages : The extraction time is long. No filtration requirement after leaching. Maintaining a relatively slightly high extraction temperature with heat from the distillation flask. When the liquid reaches the overflow level. Agitation can not be provided in the Soxhlet device to accelerate the process. The operation is repeated until complete extraction is achieved. The large amount of solvent used requires an evaporation concentration procedure. A schematic representation of a Soxhlet extractor Advantages and disadvantages of Soxhlet Extraction Advantages : The displacement of transfer equilibrium by repeatedly bringing fresh solvent into contact with the solid matrix. Solute is left in the flask and fresh solvent passes back into the plant solid bed. The possibility of thermal decomposition of the target compounds can not be ignored As the extraction usually occurs at the boiling point of the solvent for a long time 14 .SOXHLET EXTRACTOR Soxhlet extractor : a bench scale Laboratory apparatus invented in 1879 by Franz von Soxhlet. and filled with condensed fresh solvent from a distillation flask. Classical technique for the solvent extraction of nutraceuticals from plant matrices The plant material is placed in a thimbleholder. carrying extracted solutes into the bulk liquid. Also. a siphon aspirates the solution of the thimbleholder and unloads it back into the distillation flask. solute is separated from the solvent using distillation. In the solvent flask. the Soxhlet method is very simple and cheap.

Some extractors however have been used for vegetable oil extractions 15 . Kennedy extractor. Screw-Conveyor Extractors. Most of the above type extractors find applications in the metallurgical industries for ore extraction and leaching. Hildebrandt total-immersion extractor.LARGE SCALE CONTINUOUS TYPE EXTRACTORS The Bollman-type extractor. Rotocel extractor.

16 . Accelerated Solvent extraction is considered as a potential alternatives technique to SFE for extraction of polar compound. usually between 50 and 200oC and at pressures between 10 and 15 MPa Accelerated solvent extraction is form of pressurized solvent extraction that is quite similar to SFE. Technique still in experimental stages ACCELERATED SOLVENT EXTRACTION ADVANTAGES AND DISADVANTAGES OF ASE ADVANTAGES Use of non toxic extracting solvents such as carbon dioxide and water has economic and environmental benefits. there is a dramatic decrease in the amount of solvent and the extraction time for ASE DISADVANTAGES Accelerated solvent extraction performed with high extraction temperature. Compared with traditional Soxhlet extraction. which may lead to degradation of thermo labile compounds. Extraction is carried out under pressure to maintain the solvent in its liquid state at high temperature.Accelerated solvent extraction (ASE) is a solid–liquid extraction process performed at elevated temperatures.

chromatography etc. crystallization. for final recovery.g. SOLVENT FEED May be batch or continuous Mixer Settlers e. Solvent : The liquid with which the feed is contacted with. Extract : The solute rich solvent product of the operation. In liquid liquid extraction the products recovered have to be subjected to further MT operations like distillation.LIQUID LIQUID EXTRACTION SEPARATION OF A COMPONENT FROM A LIQUID MIXTURE BY TREATMENT WITH A SOLVENT IN WHICH THE DESIRED COMPONENT IS PREFERENTIALLY MORE SOLUBLE. Kerr-Mcgree Extractor SINGLE STAGE EXTRACTION EXTRACT MULTI STAGE EXTRACTION FEED SOLVENT MIXER SEPARATOR 1 RAFFINATE RAFFINATE MIXER SEPARATOR 2 MIXER SEPARATOR ‘n’ RAFFINATE SOLVENT EXTRACT EXTRACT SOLVENT EXTRACT CO-CURRENT FLOW EXTRACTION SYSTEM RAFFINATE RAFFINATE FEED MIXER SEPARATOR 1 MIXER SEPARATOR 2 MIXER SEPARATOR ‘n’ DEPLETED RAFFINATE SOLVENT SOLVENT ENRICHED WITH PRODUCT COUNTER CURRENT FLOW EXTRACTION SYSTEM Different types of liquid liquid extraction columns • • • • • Rotating Disc Contactors Perforated Plate ( Karr Column) Pulsed Plate Columns Scheibel Extractors Centrifugal Counter current “ Podbielniak Extractor” 17 . Raffinate : Residual liquid from which solute has been removed.

HORIZONTAL LIQUID LIQUID ‘PODBIELNIAK EXTRACTER VERTICAL RECIPROCATING LIQUID LIQUID EXTRACTION “ KARR” COLUMN M In Industry Solvent Extraction units for MAPs is based on ‘Soxhlet principle with recycling of solvents Basic equipments of an extraction unit consists of • Drug holders / Extractors • Solvent Storage Vessel • Reboiler Kettle • Condensers • Breather system • Infrastructure • Boiler • Refrigerated Chilling unit • Vacuum • Inert Gas LARGE SCALE SOLVENT EXTRACTION UNIT 18 .

wiped film or rotary evaporators to work under low pressures Vacuum systems with cold traps GMP Compatible : All Stainless Steel units 19 .DESIGNING A SOLVENT EXTRACTION PLANT FOR HERBS ! High Efficiency of Extraction Minimal Solvent losses IMPORTANT FACTORS WHILE Facility for cold / hot extraction SETTING UP AN Extraction with agitation EXTRACTION Multiple solvent extraction system UNIT Multiple fraction collection Online filtration unit Solvent recycling and condensing unit Vent lines with breather for minimizing solvent losses and safety Brine circulation unit Fractionating column for separation of solvent mixtures Efficient evaporating systems like falling film.

Rescinnamine Somniferum. Pods Roots Leaves Flowers Roots Roots Seeds Leaves Rhizomes Seeds Whole Pant Whole plant Rhizomes Active Constituent Artemisinin Sennosides A & B Ajmalcine. Phytosterol Xanthotoxin Di terpenoids Andrographalides Colchicine Aescin Asiaticosides Aspatic acid Baccosides Diosgenin Major Use Antimalarial Laxative Anticancer Insecticidal Hypertensive Sedative Stimulant Antiinflamatory Skin diseases Leucoderma Hepatprotective Gout.Vinblastine Vincrystine Pyrethrins Resperine.R c ered e ov S olvent Cn e er o d ns Jas neFlo ers mi w Solvent Coling o W er at T acum oV u Percolation Vessel Stea m Vacuum Concentr ator Perforated Grid Extract Line Filter Rotary Vacuum Evaporator Jasmine Concrete Absolute Alcohol Jasmine Absolute Filtratio n Chilling Plant Production of jasmine absolute using solvent extraction technique SOME IMPORTANT MEDICINAL PLANTS & THEIR ACTIVE CONSTITUENTS (That are extracted / isolated by Solvent Extraction technique) Plant Artemesia annua (Quinghasou) Cassia augustifolia (senna) Cantharanthus roseus (Periwinkle) Chyrysanthemum cinerariaefolium (Pyrethrum) Rauvolifolia serpentine Withania somniferum Ammi majus Andrographis panniculata Gloriosa superba Aesculus indica Centella asiatica Bacopa munnerai Dioscoria deltoidea Useful Plant Part Whole Plant Leaves. Rheumatism Anti inflammatory Tonic Stimulant Tonic Stimulant Steroid 20 .

SOLVENT EXTARCTION PLANT SOLVENT EXTARCTION PLANT FOR MAP’S AT BIOTECH PARK LUCKNOW 21 .

DRUG HOLDERS / EXTRACTORS 22 .

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