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Extraction techniques

  1. Compiled By R. H. Mishal Asst. Professor Sir. Dr. M. S. Gosavi College of Pharmaceutical Education & Research, Nashik.
  2.  Although, the various classes of preparations involving simple expression, aqueous hot and cold extraction and evaporation were in vogue since long time but, real and scientific rapid progress in the extraction procedures for medicinal plant preparations was made after 19th century.  Such extraction techniques and processes were highly successful in the phytochemical field leading to isolation of single pure molecules and standardized extracts for therapeutic purposes.  Simple traditional to advanced technologies conforming to official procedures are being used to manufacture different types of preparations popularly known as Galenicals. Such class of preparations includes: Decoctions  Infusions  Fluid extracts tinctures  Semi solid extracts Powdered extracts.
  3. Extracts can be defined as preparations of crude drugs which contain all the constituents which are soluble in the solvent used in making the extract. In dry extracts all solvent has been removed. Soft extracts and fluid extracts are prepared with mixtures of water and ethanol as solvent. Tinctures are prepared by extraction of the crude drug with five to ten parts of ethanol of varying concentration, without concentration of the final product.
  4.  For both extracts and tinctures the ratio drug/solvent should always be stated.  Several factors influence the extraction process.  Plant constituents are usually contained inside the cells. Therefore, The solvent used for extraction must diffuse into the cell to dissolve the desired compounds whereupon the solution must pass the cell wall in the opposite direction and mix with the surrounding liquid.  An equilibrium is established between the solute inside the cells and the solvent surrounding the fragmented plant tissues.  The speed with which this equilibrium is established depends on: • Temperature • pH • Particle size • The movement of the solvent
  5. The ideal solvent for a certain pharmacologically active constituent should: 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. 4. Have a low price. 5. Be harmless to man and to the environment. 6. Be completely volatile.
  6. Aliphatic alcohols with up to three carbon atoms, or mixtures of the alcohols with water, are the solvents with the greatest extractive power for almost all natural substances of low molecular weight like alkaloids, saponins and flavonoids. According to the pharmacopoeias, ethyl alcohol is the solvent of choice for obtaining classic extracts such as tinctures and fluid, soft and dry extracts. The ethanol is usually mixed with water to induce swelling of the plant particles and to increase the porosity of the cell walls which facilitates the diffusion of extracted substances from inside the cells to the surrounding solvent. For extraction of barks, roots, woody parts and seeds the ideal alcohol/water ratio is about 7:3 or 8:2. For leaves or aerial green parts the ratio 1:1 is usually preferred in order to avoid extraction of chlorophyll.
  7. There are many procedures for obtaining extracts like: 1. Infusion 2. Maceration 3. Percolation 4. Digestion 5. Decoction 6. Continuous hot extraction 7. Solvent-solvent precipitation 8. Liquid-liquid extraction 9. Distillation 10. Specific procedures
  8.  Infusion:Infusion: In this method, the plant material (herbal tea) is placed in a pot and wetted with cold water. Immediately afterwards, boiling water is poured over it, then left to stand, covered with a lid, for about fifteen minutes after which the tea is poured off.  Maceration:Maceration: This method is used frequently for water soluble active constituents. It consists of macerating the plant material in cold water (15-20°) for several hours.  Percolation:Percolation: In this method, the ground plant material is subjected to a slow flow of fresh solvent. 8
  9. 9 Maceration Processes General Procedure: Plant Material (Crushed or cut small or Moderately coarse powder)  Placed in a closed vessels  Whole of the selected solvent (Menstruum) added  Allowed to stand for seven days shaking occasionally  Liquid strained off  Solid residue (mark) pressed (Recover as much as occluded solution)  (Strained and expressed liquids mixed)  Clarified by subsidence or filtration  Evaporation and Concentration
  10.  Digestion:Digestion: This method is suitable for hard barks or woods which are difficult for water to penetrate. Digestion is also considered as maceration but, at a relatively elevated temperature. As aAs a general rule the temperature of the extracting medium shouldgeneral rule the temperature of the extracting medium should be in the range from 35-40be in the range from 35-40°° but not exceeding 50but not exceeding 50°°..  Decoction:Decoction: If the plant material is boiled for ten minutes or if boiling water is poured over it and allowed to stand for thirty minutes, the result is called decoction.
  11. Continuous hot extraction  Continuous hot extraction method:Continuous hot extraction method: This procedure is considered as the most common method used for the extraction of organic constituents from dried plant tissue. It can be used both on laboratory and industrial scales. In the lab, the powdered material is continuously extracted in a Soxhlet apparatus with a range of solvents of increasing polarity.  Solvent-solvent precipitation:Solvent-solvent precipitation: (I) The extract dissolved in a suitable solvent, is mixed with a less polar but miscible solvent causing the selective precipitation of the less soluble plant constituent, e.g. the precipitation of triterpenoid saponins from the methanol extract of Phytolacca dodecandra by the addition of acetone and the precipitation of gum from aqueous extracts of Olibanum by addition of alcohol. (II) By the addition of the extract to a solvent in which the constituents is insoluble or very sparingly soluble e.g. precipitation of resins from the alcoholic extracts by the addition of distilled or acidulated water. 11
  12. Liquid liquid extraction Liquid-liquid extraction, also known as solvent extraction and partitioning, is a method to separate compounds based on their relative solubilities in two different immiscible liquids, usually water and an organic solvent. It is an extraction of a substance from one liquid phase into another liquid phase. Liquid-liquid extraction is a basic technique in phytochemical laboratories, where it is performed using a separatory funnel. 12
  13. 13 Extractive Values: –Determines the amount of active constituents extracted with solvents from a given amount of medicinal plant material. Water Soluble Extractive: This method is applied to drugs which contain water soluble active constituents of crude drugs, such as tannins, sugars, plant acids, mucilage, glycosides etc. Macerate 5 g of the air dried drug, coarsely powdered, with 100 ml of chloroform water of the specified strength in a closed flask for twenty-four hours, shaking frequently during six hours and allowing to stand for eighteen hours. Filter rapidly, taking precautions against loss of solvent, evaporate 25 ml of the filtrate to dryness in a tared flat bottomed shallow dish, and dry at 105º, to constant weight and weigh. Calculate the percentage of water-soluble extractive with reference to the air-dried drug. Alcohol Soluble Extractive: This method is frequently employed to determine the approximate resin content of the drug. Macerate 5 g of the air dried drug, coarsely powdered, with 100 ml of Alcoholof the specified strength in a closed flask for twenty-four hours, shaking frequentlyduring six hours and allowing to stand for eighteen hours. Filter rapidly, taking precautionsagainst loss of solvent, evaporate 25 ml of the filtrate to dryness in a tared flatbottomed shallow dish, and dry at 105º, to constant weight and weigh. Calculate thepercentage of alcohol- soluble extractive with reference to the air-dried drug.
  14. 14 Determination of EtherSoluble Extractive : Two types of ether soluble extractives are determined for evaluation of crude drugs. The Volatile ether-soluble extractive represents volatile oil content of the drug and non-volatile ether-soluble extractives represent resin, fixed oil or colouring matter present in the drugs. Transfer a suitably weighed quantity (depending on the fixed oil content) of the air dried, crushed drug to an extraction thimble, extract with Solvent ether or petroleum ether.
  15.  The spectrum of constituents obtained by steady state extractions differs from the spectrum obtained by exhaustive extractions.  By the use of motive extraction methods, the aid of stirring and shearing forces, changes of temperature and quality of extraction solvent may lead to extracts with a spectrum of Constituents.  Different manufacturing procedures have to be assessed as equivalent if the critical quality parameters of the specification are conformed to and if compliance with standards is proven by the results of a number of production batches. 15
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