565 BOTANICAL EXTRACTS
In the extraction practice for articles of botanical origin, the constituents of interest are completely or partially separated from other components with the aid of water, alcohol, alcohol-water mixtures, or other suitable solvents. This extraction process involves the removal of the desired constituents from the plant matter with suitable menstrua, the evaporation of all or nearly all of the solvent, and the adjustment of the residual fluids, masses, or powders to the prescribed standards. Suitable inert substances may be added as carriers or diluents to improve physical characteristics. Suitable antimicrobials and other preservatives may be added to preserve the integrity. Extracts may be subjected to processes that increase the content of characterized constituents, decrease the content of unwanted constituents, or both. Extracts with no added inert substances and no processing beyond the extraction are called native extracts. In some preparations, the plant matter may be pretreated by inactivation of enzymes and microbial contaminants, grinding, defatting, or a similar procedure.
Extracts may be defined as preparations with liquid, solid, or semisolid consistency. The products obtained by extraction are fluidextracts, powdered extracts, semisolid extracts, and tinctures.
METHODS OF EXTRACTION
In the manufacture of extracts, percolation is a commonly used method. The crude material being extracted is reduced to pieces of suitable size, if necessary, then mixed thoroughly with a portion of the specified solvent, and allowed to stand for about 15 minutes. The mixture is transferred to a percolator, sufficient amount of the specified solvent is added to cover the entire solid mass, and the mixture is allowed to percolate slowly (at a rate of not more than 1 mL per minute for 1000 g of material), the matter to be extracted being always covered with a layer of solvent. The residue may be pressed, and the obtained fluid is combined with the percolate. The entire percolates are concentrated, generally by distillation under reduced pressure, so as to subject the constituents of interest in the article under extraction to as little heat as possible.
Unless otherwise specified, the crude material being extracted is reduced to pieces of suitable size, mixed thoroughly with the specified extracting solvent, and allowed to stand at room temperature in a closed container for an appropriate time, with frequent agitation until soluble matter is dissolved. The mixture is filtered, the insoluble material is washed with the same solvent used for maceration, and the filtrates are combined and concentrated, usually under reduced pressure, to the desired consistency.
fluid extracts, also known as liquid extracts, are preparations of plant matter, containing alcohol as a solvent or as a preservative, or both, and are so made that each mL contains the extracted constituents of 1 g of the crude material that it represents, unless otherwise specified in the individual monograph. They may be prepared from suitable extracts and may contain suitable antimicrobial or other preservatives.
Pharmacopeial fluidextracts are made by percolation, often following a period of maceration. The required solvent is specified in the individual monograph. The common manufacturing procedure includes concentration of the more diluted portion of percolate by evaporation or distillation under vacuum at temperatures below 60. The time of maceration and the rate of flow during percolation may be varied to adjust for the quantity and nature of the crude material under extraction, provided that the composition of the extracted constituents of interest is not adversely affected.
The rate of flow of the percolate can be slow, moderate, or rapid. With reference to the extraction of 1000 g of the starting material, at a slow rate, not more than 1 mL of percolate is produced per minute; at a moderate rate, between 1 and 3 mL per minute is produced; and at a rapid rate, between 3 and 5 mL per minute is produced. A fluidextract that tends to deposit sediment may be aged and filtered, or the clear portion may be decanted, provided that the resulting clarified liquid conforms to the Pharmacopeial standards.
powdered extracts are solid preparations having a powdery consistency obtained by evaporation of the solvent used for extraction. They may contain suitable added substances such as excipients, stabilizers, and preservatives. Standardized powdered extracts are adjusted to the defined content of constituents, using suitable inert materials or a powdered extract of the plant matter used for preparation. Where applicable, a limit for the solvent used for extraction is specified in the individual monograph.
semisolid extracts, also known as soft extracts or pillular extracts, are preparations having consistencies between those of fluidextracts and those of powdered extracts, and are obtained by partial evaporation of the solvent, water, alcohol, or hydroalcoholic mixtures being used as extracting solvents. They may contain suitable antimicrobial or other preservatives. A semisolid extract and a powdered extract obtained from the same material are interchangeable as drugs or as supplements, but each has its own advantages.
General Pharmacopeial Requirements
Unless otherwise specified in the individual monographs, Pharmacopeial requirements for the fluidextracts, powdered extracts, and semisolid extracts are as follows.
Packaging and Storage Store in tight, light-resistant containers. [noteSee Preservation, Packaging, Storage, and Labeling under General Notices and Requirements.]
Labeling Label it to indicate the name of the plant part used; the names of solvents, other than the hydroalcoholic solvents, used in preparation; the content, in percentage, of active principles or marker compounds identified in the individual monograph; and the name and concentration of any added antimicrobial or other preservative. Where active principles are unknown, the ratio of starting material to final product is stated. For semisolid extracts and powdered extracts, the identity and quantity of any added excipient is also indicated. In such cases the percentage of native extract may also be stated.
Residue on Evaporation Transfer promptly about 2 mL, accurately measured, of Fluidextract, about 0.5 g of Powdered Extract, or about 2 g of Semisolid Extract to a suitable tared, round-bottom flask. Evaporate to dryness on a water bath, and dry the residue at 100 to 105 for 3 hours. Allow to cool in a desiccator over phosphorus pentoxide, and determine the weight of the residue obtained: not less than 95% of Powdered Extract specimen remains as residue; or not less than 70% of Semisolid Extract specimen remains as residue. [note Limits for Fluidextracts are specified in the individual monographs.]
Residual Solvents If prepared with solvents other than alcohol, water, or alcohol-water mixtures, it meets the requirements for Residual Solvents 467. [noteSee ICH document Impurities: Residual Solvents for related information.]
Pesticide Residues Proceed as directed under Articles of Botanical Origin 561: meets the requirements.
Heavy Metals, Method II 231: 20 µg per g.
Alcohol Content, Method II 611 (if present): between 90% and 110% of the labeled amount of C2H5OH is found in Fluidextract and Semisolid Extract.
tinctures are liquid preparations usually prepared by extracting plant materials with alcohol or hydroalcoholic mixtures. Traditionally, tinctures of potent articles of botanical origin represent the activity of 10 g of the drug in each 100 mL of tincture, the strength being adjusted following the test for content of active principles or marker compounds. Most other plant tinctures represent 20 g of the respective plant material in each 100 mL of tincture.
Different tinctures are not always diluted to obtain the same ratio of starting plant material to final tincture. This ratio will depend on the requirements prescribed in the specific tests for content of active principles or marker compounds included in the individual monographs. As tinctures are being prepared, they are assayed in accordance with these content tests. Using the values obtained from such assays, the final concentration of a tincture is adjusted by adding more solvent or by evaporating part of the solvent.
Unless otherwise specified, tinctures are usually prepared from coarse powder or fine cuttings of plant materials either by a percolation process or a maceration process.
Carefully mix the ground mixture of ingredients with a sufficient quantity of the prescribed extracting solvent to render it evenly and distinctly damp, allow it to stand for 15 minutes, transfer it to a suitable percolator, and pack the mass firmly. Pour on enough of the specified extracting solvent to saturate the drug, and cover the top of the percolator. When the liquid is about to drip from the percolator, close the lower orifice, and allow the drug to macerate for 24 hours or for the time specified in the monograph. If the test for content of active principles or marker compounds is not required in the individual monograph, allow the percolation to proceed slowly or at the specified rate (for definitions of flow rates, see under Fluidextracts), gradually adding sufficient quantity of extracting solvent to produce 1000 mL of tincture, and mix. If a test for content of active principles or marker compounds is required, collect only 950 mL of percolate, mix, and test a portion of it as directed in the individual monograph. Dilute the remainder of the percolate with as much of the prescribed extracting solvent as calculation from the content test indicates is necessary to produce a tincture that conforms to the requirements, and mix.
Macerate the drug with 750 mL of the prescribed extracting solvent in a closed container, and put in a warm place. Agitate it frequently during 3 days or until the soluble matter is dissolved. Transfer the mixture to a filter. When most of the liquid has drained, wash the residue on the filter with a sufficient quantity of the prescribed extracting solvent, combining the filtrates, to produce 1000 mL of tincture, and mix.
general pharmacopeial requirements
Unless otherwise specified in the individual monographs, Pharmacopeial requirements for the tinctures are as follows.
Packaging and Storage Store in tight, light-resistant containers, and avoid exposure to direct sunlight and excessive heat. [noteSee Preservation, Packaging, Storage, and Labeling under General Notices and Requirements.]
Labeling Label it to indicate the name of the plant part used for preparation; the name of the solvent or solvent mixture used for extraction; and the content of the constituents of interest and the ratio of starting material to final product.
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