EXTRACTION AND RECRYSTALLIZATION (EXPT 3) Flashcards
A process that selectively dissolves one or more compounds into an appropriate solvent.
Extraction
The resulting solution from extraction is called an ?
Extract
Refers to the transfer of compounds from one liquid solvent to another one.
Extraction
Can be used to separate unwanted impurities or to separate mixtures of compounds.
Extraction
The two solvents for extraction must be?
Immiscible
Can be defined as preparations of crude drugs which contain all the constituents which are soluble in the solvent.
Extracts
Solid residue obtain after extraction.
Marc
Solvent used for extraction.
Menstruum
Extraction is to _______ a compound from one layer to another.
pull out
A compound partitions more toward where it is more _____ (equilibrium).
Soluble
A compound partitions more toward where it is more _____ (equilibrium).
Soluble
_______ extractions may be needed to completely extract a substance.
Multiple
Parts of separatory funnel
- stopcock
- solute in organic phase
- solute in aqueous phase
Factors affecting extraction process
- Nature of drug
- Solvent
- Temperature
- pH
- Particle size
Methods of Extraction
- Infusion
- Decoction
- Digestion
- Maceration
- Percolation
- Continues hot extraction
Fresh _____ are prepared by macerating the crude drug for a short period of time with cold or boiling water.
Infusion
These are dilute solutions of the readily soluble constituents of crude drugs.
Infusion
Types of Fresh Infusion
- Fresh Infusion
- Concentrated Infusion
Fresh Infusion example
Infusion of Orange
Concentrated Infusion example
Concentrated infusion of Quassia
In this process, the crude drug is boiled in a specified volume of water for a defined time; it is then cooled and strained or filtered.
Decoction
This procedure is suitablr for extracting water-soluble, heat stable constituents.
Decoction
Example of this procedure is Tea & Coffee.
Decoction
A form of maceration in which gentle heat is used during the process of extraction.
Digestion
It is used when moderately elevated temperature is not objectionable.
Digestion
The solvent efficiency of the menstruum is thereby increased.
Digestion
Example of this procedure is Extraction of Morphine.
Digestion
In this process, solid ingredients are placed in a stoppered container with the whole of the solvent and allowed to stand for a period of at least 3 days (3 - 7 days) with freuqent agitation, until soluble matter is dissolved.
Maceration
The mixture is then strained (through sieves / nets), the marc pressed and the combined liquids clarified (cleaned by filtration) or by decantation, after standing.
Maceration
It is continuous downward displacement of the solvent through the bed of crude drug material to get extract.
Percolation
Most frequently used to extract active ingredients in the preparation of tinctures and fluid extracts.
Percolation
It is the method of short successive maceration or process of displacement
Percolation
A percolator (a narrow, cone-shaped vessel open at both ends) is generally used.
Percolation
Steps in Percolation
- Size reduction
- Imbibition
- Packing
- Maceration
- Percolation
Continuous extraction of a component from a solid mixture.
Soxhlet Extractor
Boiling solvent vapors rise up through the larger side- arm.
Condensed drops of solvent fall into the porous cup, dissolving out the desired component from a solid mixture. When the smaller side-arm fills to overflowing, it initiates a siphoning action.
The solvent, containing the dissolved component, is siphoned into the boiler below residual solvent then drains out of the porous cup, as fresh solvent drops continue to fall into the porous cup. and the cycle repeats.
Soxhlet Extractor
Used in separation of immiscible liquids.
Separatory Funnel
Separatory Funnel Flowchart
Extract > Separate > Dry > Evaporate
A liquid substance capable to dissolve other substances (solutes) without chemical changes.
Solvent
Molecular structure of solvents
Inorganic solvents
Organic solvents
Types of solvents
Ability of a substance to dissolve another substance is determined by compatibility of their molecular structures (like dissolves like).
Molecular Structure of Solvents
Polar Protic Solvents
Dipolar Aprotic Solvents
Non-polar Solvents
Types of Molecular Structure of Solvents:
A polar protic molecule consists of a polar group OH and a non-polar tail.
The structure may be represented by a formula R-OH. Polar protic solvents dissolve other substances with polar protic molecular structure.
Polar Protic Solvents
Polar protic solvents are miscible with _____ (hydrophilic).
Water
Examples of ______________: water (H-OH), acetic acid (CH3CO-OH)methanol (CH3-OH), ethanol (CH3CH2-OH), n-propanol (CH3CH2CH2-OH), n-butanol (CH3CH2CH2CH2-OH).
Polar Protic Solvents
Molecules possess a large bond dipole moment (a measure of polarity of a molecule chemical bond).
They do not contain OH group.
Dipolar Aprotic Solvents
Examples of ___________: acetone (CH3)2C=O, ethyl acetate (CH3CO2CH2CH3), dimethyl sulfoxide (CH3)2SO, acetonitrile (CH3CN). dimethylformamide (CH3)2NC(O)H.
Dipolar Aprotic Solvents
Are hydrophobic (immiscible with water).
Are liphophilic as they dissolve non-polar substances such as oils, fats, greases.
Non-polar solvents
Examples of ___________: carbon tetrachloride (CCI4), benzene (C6H6), and diethyl ether (CH3CH2OCH2CH3), hexane methylene chloride (CH2Cl2). (CH3(CH2)4CH3),
non-polar solvents
The most popular inorganic (not containing carbon) solvents are ?
Water (H2O), and aqueous solutions containing special additives (surfactants, detergents, PH buffers, inhibitors).
Other __________ are liquid anhydrous Ammonia (NH3), concentrated sulfuric acid (H2SO4), sulfuryl chloride fluoride (SO2CIF).
Inorganic solvents
A type of volatile organic compound (VOC).
Organic Solvent
Are organic chemicals which vaporize at room temperature.
VOCs (Volatile Organic Compounds)
__________ are useful for dissolving certain materials and substances.
__________ are often used in the manufacture of pharmaceutical products, footwear, paints, varnishes and adhesives.
Organic Solvents
Types of ______ compounds used as solvents include: Aromatic compounds, eg benzene and toluene
Alcohols, eg methanol
Esters and ethers
Ketones, eg acetone
Amines
Nitrated and halogenated hydrocarbons
Organic
Two immiscible solvents:
- A polar one (frequently water)
- Nonpolar one (an organic solvent)
Nonpolar hydrocarbons and ethers (polar) are ____ dense than water, so the water tends to move to the bottom.
Less
Most chlorinated solvents are ____ dense than water, so the water will be on top.
More
- Be highly selective for the compound to be extracted.
- Not react with the extracted compound or with other compounds in the plant material
- Have a low price.
- Be harmless to man and to the environment.
- Be completely volatile.
6.. Should not mix up with water. - Should have the big capacity in relation to extractive.
- The density of solvent should be difference from water density.
- Should have the minimum viscosity.
Ideal Properties of the Solvents
Defined as a drug because it stimulates the central nervous system, causing increased alertness.
Caffeine
This gives most people a temporary energy boost and elevates mood.
This is in tea, coffee, chocolate, many soft drinks, and pain relievers and other over- the-counter medications.
Caffeine
Caffeine is soluble in water, but is more soluble in _____.
DCM
Title of Experiment #3?
Extraction and Recrystallization