rexresearch.com
rexresearch.com
Lactucarium / Lettuce Opium
https://en.wikipedia.org/wiki/Lactucarium
Lactucarium
Lactucarium is the milky fluid secreted by several species of lettuce, especially Lactuca virosa, usually from the base of the stems. It is known as lettuce opium ...
Uses -- Analgesic, sleep aid, euphoriant
Source plant(s) -- Lactuca spp
Part(s) of plant -- Latex (see also seeds)
Geographic origin -- Southern Europe
https://www.youtube.com/watch?v=SArqxKInNB0
Lettuce Opium - Sticky extract of wild lettuce, Lactuca virosa
Lactuca virosa
Young plants of giant wild lettuce are a good ingredient for heroic salads. This is the most cold hardy of all lettuces, germinates in the fall and grows very nicely through the winter in a zone 7, producing very reasonable salads midwinter, which is before the plant goes tough and bitter. Lactuca virosa is a preferred wild species from Europe–nutrient dense, good winter salad, bright purple-black seeds, much less spiny than the new world weedy types. Mature plants contain high concentrations of bitter, rubbery sap, which when milked from the plant and dried is known as lactucarium. So concentrated, the sap is mildly sedative, antitussive, and analgesic. Origination: Native to Central and Southern Europe. Recommended Uses: Mature plants contain high concentrations of bitter, rubbery sap, which when milked from the plant and dried is known as lactucarium. So concentrated, the sap is mildly sedative, antitussive, and analgesic. Height: Up to 6 feet tall Flower Color: Green Uses: Salads Organically Grown Sowing Instructions Surface sow seeds into flats of moist soil, pressing lightly and keeping moist for germination in 7-14 days keeping seeds at 70 degrees Fahrenheit. Keep in partial sun until germination transplanting to full sun
https://www.wildlettuce.com/lactucashop/lettuce-opium-sticky-extract-of-wild-lettuce.html
Sticky Extract of Lactuca Virosa
Lettuce opium is the holy grail of wild lettuce products! The medicinal name for lettuce opium is lactucarium, we're just calling it sticky extract for the time being. It came into pretty big production in the 19th century in Aubière, France. The method developed by the pharmacist H. Aubergier involved employing the women of the village to cut the plants and harvest the sap by hand. These days it's done by a tailored extraction using water and alcohol in a modern laboratory. THIS IS GENUINE LACTUCA VIROSA EXTRACT, NOT CHEAP AND FAKE CHINESE EXTRACT
https://backwaterbotanics.wordpress.com/2015/04/14/wild-lettuce-lactuca-virosa/
Wild lettuce is a small, biennial herbaceous plant in the Asteraceae family found throughout Europe, Southeast England, the Punjab region of Pakistan, Australia, and the Southeastern United States along roadsides and in open fields. It has a central erect hollow stem that is a typically smooth and pale green, sometimes spotted with purple, from which a rosette of broad spiny leaves grow. The plant starts as a low-lying rosette, but in the summer when it goes to flower and seed bolts into a spindly upright plant. There are a few prickles on the lower parts of the plant and on the short horizontal branches above. The numerous, large, radical leaves are from 6 to 18 inches long, entire, and obovate-oblong. The rough, black fruit is oval, with a broad wing along the edge, and prolonged above into a long, white beak carrying silvery tufts of hair. The plant has a brown tap-root and summer blooming clusters of pale yellow composite flowers. Its harvested when in full bloom in the late summer and stored best juiced, dried, or prepared in a tincture. It’s easily cultivated in the garden in well drained, moist soils in full sun. The whole plant is rich in a bitter, milky juice that flows freely from any wound. When dry, it hardens, turns brown, and is known as lactucarium.
Parts Used
Fresh leaves, Latex sap
Medicinal Uses
Wild Lettuce is a non-addictive sedative, antitussive, anodyne, mild psychotropic, and hypnotic herb, most commonly used to treat insomnia, restlessness, anxiety, over-active nervous systems, and excitable children. It’s anti-spasmodic properties can be useful in treating whooping cough as well as soothing other coughs. It also relieves muscular pains associated with rheumatic arthritis, as well as colic pain in the guts and uterus, making it a good choice when treating menstrual cramps. The plant is best used fresh, preferably juiced, which can be either taken immediately or dehydrated for storage. The dried leaf has value, but it loses most of its pain relieving qualities when dried. However, dried, it still acts as a mild sedative that can help with pain and sleep, especially when combined with other herbs.
Folk Uses
Once commonly known as “Lettuce Opium”, Wild Lettuce was a common sedative. It was smoked to induce a dreamy, hypnotic state that was milder and less addictive than opium. Dioscorides, an 1st century physician, noted Wild Lettuce had similar effects to that of the opium poppy, and in a concentrated state, was a strong hallucinogen. It was mixed with mother’s milk to soothe burns, and cooked in any type of milk as a home remedy for arthritis. Boiled with rose, it made a useful compress for easing headaches. It was also considered an anaphrodesiac, commonly applied as a compress with camphor to the testicles to repress sexy dreams. A decoction of the leaves was also used as a face wash. In Assyrian herbal medicine, wild lettuce seeds were used with cumin as a poultice for soothing the eyes. It was brought to the United States from Europe supposedly as an adulterant for opium.
Flavor Profile and Energetics
Bitter, cooling
Dosage
As an infusion, 1-2 teaspoons of the dried leaves per cup of boiling water, steeped for 10-15 minutes. As a tincture, 2-4ml three times a day.
Combinations
For irritable coughs, combine with wild cherry bark or licorice. For insomnia and restlessness, combine with valerian and pasque flower, or other pleasant tasting nerviness such as chamomile, lavender, and mint.
Contraindications
Pregnant women and individuals with glaucoma and prostate enlargement should avoid this herb. Ingesting very large quantities can result in stupor, difficulty breathing, coma, and in extreme cases, death. This herb should be avoided two weeks before undergoing any surgery due to possible complications with anesthesia. Allergic reactions in individuals that are sensitive to ragweed are possible.
CN102659868
Extracting and purifying method for Macrocliniside A
The invention relates to an extracting and purifying method for Macrocliniside A. The extracting and purifying method is characterized by comprising the steps of adopting supercritical CO2 to extract fibrous root of lactuca virosa, enabling acetone to serve as entrainer, collecting extract and dispersing the extract in water, carrying out high-pressure silicagel column chromatography, adopting petroleum ether-acetone to perform gradient elution, collecting each elution part, then performing thin-layer chromatography, collecting components containing Macrocliniside A, forming extract by concentration, utilizing methanol to disperse the extract, performing purification through preparative liquid chromatograph, utilizing methanol aqueous solution to perform elution, concentrating target components, and obtaining Macrocliniside A by drying. According to the method, the conditions are mild, adverse effects on product activities caused by partial high temperature in a traditional method are avoided, the process is reasonable, rapid extraction, separation and purification can be achieved, and industrialization is easy.
DESCRIPTION
The invention relates to a method for extracting and purifying large chrysoside A, characterized in that the lettuce is used as the entrainment agent and the extract is collected and dispersed in water. The mixture is subjected to high pressure silica gel column chromatography, - acetone gradient elution, collecting the eluted fraction, and then carrying out thin layer chromatography, collecting the components containing the big testosterone A, concentrated into the extract and then dispersed with methanol, the preparation of liquid chromatography for purification, methanol aqueous solution Elute and concentrate the target component. The method has the advantages of mild condition and avoids the adverse effect of the local high temperature on the activity of the product. The process is reasonable and can be quickly extracted, separated and purified, and it is easy to be industrialized.
Technical field
The present invention belongs to the field of Chinese medicine and pharmaceuticals, and relates to a method for extracting and purifying large testosterone.
Background technique
(Macrocliniside A), molecular formula C21H28O9, molecular weight 424.45, is from Compositae (Compositae) fried lettuce Lactuca virosa L. The sesquiterpene compounds are isolated from the roots. Pharmacological studies have shown that metoclathomide A has a cytotoxic effect on the L-5178Y cell line ID50 is 21.4µg / ml.
At present, there is no report about the extraction and preparation of the test system, so it is a kind of extraction and purification method of the big testosterone A, which provides a rich material basis for the development and utilization of the lettuce resources and the pharmacological research.
The contents of the invention
The present invention aims at overcoming the above-mentioned technical defects and providing a method for extracting and purifying meta-inosine A, which has a good separation effect, a high yield, a good product purity and is suitable for industrial production.
In order to achieve the above object, the present invention adopts the following technical scheme:
The method comprises the following steps: using the supercritical CO2 extraction and acetone as the entrainment agent, collecting the extract, dispersing in water, carrying out high pressure silica gel column chromatography, using petroleum ether- Acetone gradient elution, collecting the eluted fraction, and then carrying out thin layer chromatography, collecting the components containing big testosterone A, concentrated into an extract and then dispersed with methanol, purified by preparative liquid chromatography, methanol aqueous solution for washing The target component is concentrated and dried to obtain the big testosterone.
The supercritical CO2 extraction conditions are as follows: the extraction kettle pressure is 18-35MPa, the extraction kettle temperature is 33-55 ° C, and the extraction time is 2-5h.
The column pressure of the high-pressure silica gel column is 2.2-3.1MPa, the column diameter is 150-250mm, the column diameter ratio is 1: 12-20, and the silica mesh number is 100-400 mesh.
The methanol aqueous solution has a concentration of 25-29%.
The invention has the advantages that:
1 -- The method has the advantages of supercritical extraction, column chromatography and preparation of liquid phase separation, and has the advantages of short time, high yield, simple operation and easy industrial production.
2 -- Using high pressure column chromatography, the amount of large sample, short cycle, good separation, high purity products.
3 -- The invention provides the pharmacological raw material, the theory and the practice support for the further development and utilization of the big testosterone A.
The present invention is further illustrated by the following examples, but is not intended to limit the scope of the invention.
Detailed description
Example 1:
The extraction temperature was 38 ° C, the extraction pressure was 25MPa, the flow rate of CO2 was 4ml / g crude drug / min, the pressure was kept and the temperature was kept constant, and 500ml acetone was added into the supercritical CO2 extraction kettle. As a entrainer, the extraction time was 4h, the separation kettle temperature was 25 ° C and the pressure was 6 MPa. The analytical extract was collected and dispersed in water and loaded onto a 200-300 mesh silica column. The column pressure of the high pressure column was 2.9 MPa, column diameter of 150mm, column diameter ratio of 1:18, with petroleum ether - acetone mixed solvent, followed by volume ratio of 1: 1: 1: 1, 6, 1: 12 elution, The mobile phase consisted of 25% methanol aqueous solution at a flow rate of 15 ml / min, and the mobile phase was prepared by the following steps: (1) Detection wavelength: 231nm, the target component was concentrated, dried to obtain 98.9% purity of protestin A7.5g.
Example 2:
The extraction temperature was 35 ° C, the extraction pressure was 18MPa, the CO2 flow rate was 5ml / g crude drug / min, the kettle pressure was kept and the temperature was constant, and the temperature was changed to 600ml acetone As the entrainer, the extraction time was 4h, the separation kettle temperature was 25 ° C and the pressure was 7MPa. The analytical extract was collected, dispersed in water and loaded onto the 100-200 mesh silica gel column. The column pressure of the high pressure column was 3.1 MPa, the column diameter is 250mm, the column diameter ratio is 1:20, the petroleum ether - acetone mixed solvent, followed by the volume ratio of 1: 1: 1: 4, 1: 11 elution, The mobile phase consisted of 29% methanol aqueous solution at a flow rate of 20 ml / min, and the mobile phase was prepared by the following method. The mobile phase was prepared by the following steps: Detection wavelength: 231nm, concentrated target components, drying that was 98.7% purity of the large testosterone A6.8g.
Example 3:
The extraction temperature was 55 ° C, the extraction pressure was 35MPa, the flow rate of CO2 was 4ml / g crude drug / min, the pressure was kept and the temperature was constant, and the temperature was changed to 1200ml acetone. The extraction temperature was 55 ?, As the entrainer, the extraction time was 4h, the separation kettle temperature was 40 ° C and the pressure was 6.5MPa. The analytical extract was collected and dispersed in water to the 300-400 mesh silica column. The column pressure of the high pressure column was 2.2MPa, column diameter of 200mm, column diameter ratio of 1:15, with petroleum ether - acetone mixed solvent, followed by volume ratio of 1: 2,1: 6,1: 12 elution, sub-collection of each The mobile phase consisted of 26% methanol aqueous solution, flow rate: 35ml / min. The mobile phase was prepared by the following method. The mobile phase was prepared by the following steps: mobile phase: 26% methanol aqueous solution, flow rate: 35ml / min , Detection wavelength: 231nm, concentrated target components, drying that was 98.8% purity of the big testosterone A14.6g.
Example 4:
The extraction temperature was 40 ° C, the extraction pressure was 25MPa, the CO2 flow rate was 3.5ml / g crude drug / min, the pressure was kept and the temperature was constant, and the temperature was changed to 900ml Acetone as entrainer, the extraction time was 4h, the separation kettle temperature was 30 ° C and the pressure was 7MPa. The analytical extract was collected and dispersed in water and loaded onto a 200-300 mesh silica column. The column pressure was 2.6MPa, the inner diameter of the column is 220mm, the column diameter ratio is 1:15, the petroleum ether-acetone mixed solvent is sequentially eluted according to the volume ratio of 1: 1, 1: 5, 1: 11, The mobile phase consisted of 27% methanol aqueous solution at a flow rate of 50 ml / min. The mobile phase consisted of a liquid phase: the mobile phase consisted of: , Detection wavelength: 231nm, concentrated target components, drying that was 98.6% purity of the big testosterone A10.2g.
GB483789
A process for the production of a stable, water-soluble medicament from the latex of lactuca virosa
A stable water-soluble product is obtained from the latex of lactuca virosa by separating the freshly gathered latex into a liquid portion and an inactive solid portion. The latex is preferably mixed with water and then separated by filtering, centrifuging &c. The liquid portion may be stabilized by addition of reducing agents or acids, e.g sulphurous acid, sodium bisulphite, formaldehyde, tartaric acid, citric acid and also by destroying the oxydases by heating to 80 DEG C. Preservatives may be added for preventing the formation of mould. The liquid product may be evaporated to dryness.
The desiccated latex of Lactuca virosa, known as Lactucarium, is an old popular remedy, which was formerly employed, on account of its mild narcotic action, for subduing coughs, spasmodic coughs, insomnia and asthma.
Commercial lactucarium can be obtained by collecting, in a basin, the latex issuing after a cross cut has been made through a shoot After standing for about a day, the coagulated sap is removed from the basin and slowly dried in the air or by slightly warming The lactucarium is then obtained as a viscid mass, in the form of spherical segments, dark brown on the outside and grey to yellowish-white inside.
The fresh, fluid latex has the following approximate composition:
by weight Water 78 % Constituents soluble in water 10 % Do insoluble do 12 % In Pharmacy, lactucarium was usually employed by being triturated and brought into the condition of an emulsion This lactucarium and its preparations were recommended in numerous medical publications, so that, formerly, it was widely used On the other hand, the entire inefficacy of the product was set forth in other publications This uncertainty of action led to lactucarium being displaced progressively by the more reliable opium and its preparations; and it has now practically disappeared from the pharmacopeia.
Exhaustive experiments have now shewn that the decline and irregularity in the action of lactucarium is due to the following causes:
( 1) The active substancees are destroyed by oxidation in the air.
( 2) The destruction is accelerated by oxydases which are present, in a high state of concentration, in the latex.
( 3) The destruction is also accelerated 55 by the existing method of preparation, the removal of the water being effected in the presence of the substances which are insoluble in water, whilst, at the same time, the water-soluble, but active 60 substances are carried towards the outside, by the water migrating to the surface In this manner, the concentration of active substances in the lactucarium diminishes from the interior 65 outwards, the composition, therefore, becoming irregular; and, moreover, the active substances, susceptible to oxidation, accumulate at the surface and are, therefore, particularly exposed to rapid 70 destruction The destruction is further accelerated because, by reason of its high sugar content ( 4 %), tile lactucarium forms a good nutrient subtratum for mould fungi, and falls a prey to mould 75 and rot These perceptions have led to the new process forming the subject of the present Application.
It has been proposed to treat the expressed juice of lactuca virosa by heat 80 ing it to 95 ' so as to remove solid albuminous material and to evaporate the water soluble portion to obtain a soft extract.
It has been ascertained, however, that 85 all the active constituents of the latex of lactlca virosa can be recovered, with certainty, in a stable, unitform and watersoluble state by separating tile freshly coagulated (or only a few days old) latex 90 into a solution containing all the active substances, and a solid, inactive portion, followed by preventing the destruction of the active substances by an addition of reducing agents 95 For this purpose, and in accordance with the present invention, the fresh latex is preferably mixed with water and then separated, by filtration, centrifuging or the like, into an active solution and a 100 solid, inactive portion.
If, instead of being immediately dried, as in the old method of preparation, the fresh latex be protected against loss of water through evaporation, by closing 105 the collecting vessel, a spontaneous 483,789 separation into an aqueous solution and a solid component occurs after coagulation In such event, the aqueous solution containing all the active substances can -5 be separated from the solid, inactive substances by aspiration, centrifuging, pressing and washing.
The resulting product can be rendered permanently stable by an addition of reducing agents, or acids, such as sulphurous acid, sodium bisulphite, formaldehyde, tartaric acid, citric acid and the like.
The product may also be stabilised by destroying the contained oxydases by warming the solution to 800 C, the time required varying in accordance with the oxydase content.
For subduing mould fungi, a preservative, su ch as aminobenzaic acid, salicylic acid, and the like, may be added to the solutions.
By the new process, the whole of the active constituents of the latex of Lactuca virosa are obtained in the form of a perfectly homogeneous stable, dry and water-soluble powder, which is free from all ballast substances retarding resorption The amount of the eliminated inactive substances is more than half the dry weight.
This product also represents a great improvement for the pharmaceutical technique of the further working up into therapeutic preparations, because:
( 1) The active substances are present in water-soluble form, ( 2) The removal of the inactive substances could enable the therapeutic doses to be reduced by more than one half, a point of considerable importance in the manufacture of tablets.
( 3) Uniform dosing can be attained reliably; ( 4) The active substances are perfectly stable in storage.
EXAMPLE 1.
The latex, issuing after incising the plants, is stripped off into a vessel containing water, sulphbrous acid or a solution of sodium bisulphite, tartaric acid or citric acid The latex coagulates and is separated, by filtration, aspiration or pressing, into a solution containing all the active substances, and a solid, inactive portion The residual portions of solution contained in the solid portion are extracted by washing.
EXAMPLE 2.
The latex, issuing, after incising the 60 plants, is collected in a vessel adapted to be closed, such as a bottle or jar with a capacity of about 100-200 cc When full, the vessel is closed, thereby preventing evaporation of the water After 65 standing for about a day, spontaneous separation into a solid and a liquid portion occurs The spontaneously separated solution, which contains the active substances, is separated from the solid, 70 inactive constituents by aspiration, pressing, filtration and washing.
For the purpose of destroying the oxydases, the resulting solution is heated to about 80 C until no oxydases are any 75 longer detectable by the Whitby method (Kolloid Zeitschrift, vol 12 ( 1913), p 149), after which it is evaporated to dryness.
