Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev

Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev

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3 MACERATION, PERCOLATION AND INFUSION TECHNIQUES FOR THE EXTRACTION OF MEDICINAL AND AROMATIC PLANTS thermore, if the dry powder is packed, fine particles may be washed down the column and settle at the lower levels, reducing the porosity drastically, blocking the column and making the column nonuniform. The finer particles may even be washed out of the column. These difficulties can be prevented by a preliminary uniform moistening of the raw material with the menstruum for a period of 4 h in a separate closed vessel; this process is called imbibition. During this period, the crude drug is allowed to swell to the maximum extent. Hence, when aqueous solvents are used for extraction, more menstruum is needed during imbibition. Also, the occluded air in the drug powder is replaced by the vapor of the solvent, thereby enabling the material to be more evenly packed and allowing the menstruum to flow more uniformly. Uneven packing permits more solvent to pass through channels offering less resistance to the flow of the solvent, thus resulting in inefficient extraction. After imbibition, the drug is packed evenly into the percolator. The imbibed drug is packed over a loose plug of tow or other suitable material previously moistened with the solvent. Even packing can be achieved by introducing the material layer by layer and pressing it with a suitable implement to give even compression; the pressure exerted on the material depends on the nature of the material and its permeability. After packing is over, a piece of filter paper is placed on the surface followed by a layer of clean sand such that the top layer of the drug is not disturbed when solvent is added for extraction. Sufficient menstruum is now poured over the drug slowly and evenly to saturate it, keeping the tap at the bottom open to allow the occluded gases between particles to pass out. Menstruum should never be poured with the tap closed since the occluded air will escape from the top, disturbing the bed. When the menstruum begins to drip through the tap, the tap is closed; sufficient menstruum is added to maintain a small layer above the drug and allowed to stand for 24 h. The layer of menstruum above the surface of the bed prevents drying of the top layer, which may result in the development of cracks on the top surface of the bed. The 24-h maceration period allows the solvent to diffuse through the drug, solubilize the constituents and leach out the soluble material. In this way, the extraction is more efficient than carrying out percolation without the maceration period. After the maceration, the outlet is opened and the solvent is percolated at a controlled rate with continuous addition of fresh solvent. The volume of percolate collected depends on the nature of the final product. In general, about 75% of the volume of the finished product is collected, the marc is pressed and the expressed liquid is added to the percolate, giving about 80%-90% of the final volume. After assay, the volume is adjusted with calculated quantities of fresh menstruum. If no assay is available, the volume is adjusted after adding the other constituents, if any. In percolation, the expressed liquid is devoid of active constituents as they are already extracted during the percolation period; pressing the marc is only to recover the valuable solvent. This is in contrast with maceration in which the marc is pressed. 76

EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS 3.6.2 Modifications to the General Process of Percolation In the general process of percolation, particularly in the manufacture of concentrated preparations like liquid extracts, the following problems may arise: • If the active substances are thermolabile, evaporation of large volumes of dilute percolate may result in partial loss of the active constituents. • In the case of alcohol-water mixtures, evaporation results in preferential vaporization of alcohol, leaving behind an almost aqueous concentrate. This may not be able to retain the extracted matter in solution and hence the substances may precipitate. In such cases, the general process of percolation is modifi ed, as described in the next paragraphs. 3.6.2.1 Reserved Percolation In this case, extraction is done through the general percolation procedure. At the end, the evaporation is done under reduced pressure in equipment like a climbing evaporator to the consistency of a soft extract (semisolid) such that all the water is removed. This is then dissolved in the reserved portion, which is strongly alcoholic and easily dissolves the evaporated portion with any risk of precipitation. 3.6.2.2 Cover and Run Down Method This is a process that combines the maceration and percolation techniques. This process cannot be used for materials that contain volatile principles or for those which undergo change during the evaporation stage. This procedure is advantageous because industrial methylated spirit may be used for extraction instead of the costly rectifi ed spirit. The detailed procedure is as follows. After the imbibition stage, the material is packed in a percolator and macerated for a few hours with a suitable diluted industrial methylated spirit. Then, the liquid is run off and the bed is covered with more menstruum. Maceration is done as before and the second volume of the extract is collected. This process is repeated several times with the later weaker extracts used for extraction of a fresh batch of the drug. More concentrated fractions are evaporated under reduced pressure to eliminate the toxic methanol. After the concentrate is assayed for the active principle or for total solids content, it is diluted with water and ethanol to obtain the correct concentration of alcohol and active principle. 77

EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS<br />

3.6.2 Modifications to the General Process of Percolation<br />

In the general process of percolation, particularly in the manufacture<br />

of concentrated preparations like liquid extracts, the following problems<br />

may arise:<br />

• If the active substances are thermolabile, evaporation of<br />

large volumes of dilute percolate may result in partial loss<br />

of the active constituents.<br />

• In the case of alcohol-water mixtures, evaporation results<br />

in preferential vaporization of alcohol, leaving behind an almost<br />

aqueous concentrate. This may not be able to retain<br />

the extracted matter in solution <strong>and</strong> hence the substances<br />

may precipitate.<br />

In such cases, the general process of percolation is modifi ed,<br />

as described in the next paragraphs.<br />

3.6.2.1 Reserved Percolation<br />

In this case, extraction is done through the general percolation<br />

procedure. At the end, the evaporation is done under reduced pressure in<br />

equipment like a climbing evaporator to the consistency of a soft extract<br />

(semisolid) such that all the water is removed. This is then dissolved in the<br />

reserved portion, which is strongly alcoholic <strong>and</strong> easily dissolves the evaporated<br />

portion with any risk of precipitation.<br />

3.6.2.2 Cover <strong>and</strong> Run Down Method<br />

This is a process that combines the maceration <strong>and</strong> percolation<br />

techniques. This process cannot be used <strong>for</strong> materials that contain<br />

volatile principles or <strong>for</strong> those which undergo change during the evaporation<br />

stage. This procedure is advantageous because industrial methylated spirit<br />

may be used <strong>for</strong> extraction instead of the costly rectifi ed spirit.<br />

The detailed procedure is as follows. After the imbibition stage,<br />

the material is packed in a percolator <strong>and</strong> macerated <strong>for</strong> a few hours with a<br />

suitable diluted industrial methylated spirit. Then, the liquid is run off <strong>and</strong> the<br />

bed is covered with more menstruum. Maceration is done as be<strong>for</strong>e <strong>and</strong> the<br />

second volume of the extract is collected. This process is repeated several<br />

times with the later weaker extracts used <strong>for</strong> extraction of a fresh batch of the<br />

drug. More concentrated fractions are evaporated under reduced pressure to<br />

eliminate the toxic methanol. After the concentrate is assayed <strong>for</strong> the active<br />

principle or <strong>for</strong> total solids content, it is diluted with water <strong>and</strong> ethanol to obtain<br />

the correct concentration of alcohol <strong>and</strong> active principle.<br />

77

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