CN1634295A - Preparation method for climbing nightshade extract - Google Patents
Preparation method for climbing nightshade extract Download PDFInfo
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- CN1634295A CN1634295A CN 200410051623 CN200410051623A CN1634295A CN 1634295 A CN1634295 A CN 1634295A CN 200410051623 CN200410051623 CN 200410051623 CN 200410051623 A CN200410051623 A CN 200410051623A CN 1634295 A CN1634295 A CN 1634295A
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- herba solani
- solani lyrati
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Abstract
The invention provides a preparation method for climbing nightshade extract which comprises, steeping medicinal powders with edible ethanol, decompression reclaiming ethanol and compensating the soak, charging natural clarifying agent so as to precipitate the impurity, finally drying the filtered clean liquid into block-shaped solid extract, wherein the major component of the extract is steroidal alkaloid with anti-inflammation action, which can be prepared into electuary for treating eczema and fungus skin diseases.
Description
Affiliated technical field
The present invention relates to a kind of extracting method of plant extract, the preparation method of a kind of plant of Solanaceae Herba Solani Lyrati extract of more specifically saying so.
Background technology
Herba Solani Lyrati (Solanum Lyratum Thumb) is the Solanaceae platymiscium, and the commercial name of an article has Herba Solani Lyrati, and another name has Yangquan, another name for Sichuan Province, Herba Solani Lyrati, Hu Mao Teng etc.Herba Solani Lyrati is the medical material in China's pharmacopeia, the normal Herba Solani Lyrati treatment tumor that adopts in traditional medicine, and generally do not use separately, relevant document record only comes across in the compound recipe, the extracting method of its active ingredient is a decocting, up to now, do not see the report of Herba Solani Lyrati active ingredient steroid alkaloid extracting method as yet.
Summary of the invention
Herba Solani Lyrati contains steroid alkaloid, and as tomatidine (Tomatidine), solasodine (Solasodine) and dioscin (Dios restrains enin), these steroid alkaloids have antibacterial activity, and wherein the effect of tomatidine is stronger.The objective of the invention is to remedy the deficiency of prior art, the preparation method of the plant of Solanaceae Herba Solani Lyrati extract that a kind of technology is comparatively simple, cost is low and the product recovery rate is bigger is provided, the steroid alkaloid of Herba Solani Lyrati is applied on the medicine.
The preparation method of this plant of Solanaceae Herba Solani Lyrati extract comprises the step of following order:
(1) with 1 part of Herba Solani Lyrati pulverizing medicinal materials, add 8~13 parts of edible ethanols and soak post-heating to 60~85 ℃ insulation in 0.8~1.2 hour 40~70 minutes, filtered while hot is emitted soak for the first time subsequently, then add 4~7 parts of edible ethanols and be heated to 60~85 ℃ of insulations 40~70 minutes toward medicinal residues, filtered while hot goes out soak for the second time, and last past again medicinal residues add 3~6 parts of edible ethanols and obtain soak for the third time with same heating-up temperature and temperature retention time;
(2) three soaks that step (1) is obtained combine, and adopt the decompression method to reclaim ethanol, and soak is concentrated into 4~6 parts;
(3) under well-beaten situation, add two kinds each 0.01~0.012 part of natural clarifying agent A and B, leave standstill and be no less than 10 hours soak is fully precipitated, filter then and remove precipitation, add again and be not more than 0.1 part of clear water washing precipitation, filtering the back adds in the soak, the immersion clear liquid that is obtained adopts the decompression method to concentrate, and is dried to the blocks of solid extract under vacuum condition.
The umber that is adopted in preparation method of the present invention is a weight portion.
Edible ethanol of the present invention is the edible ethanol of 30% concentration.
After the Herba Solani Lyrati concentrated solution that the present invention's (2) step obtains, can add 0.01~0.012 part of medical activated carbon, to put coldly after the stirring, purpose is to remove pigment.
The edible ethanol that the present invention added is comparatively suitable with 8~13 parts, crosses that I haven't seen you for ages extracts not exclusively the active ingredient of Herba Solani Lyrati, and the dissolution rate of active ingredient improves not obviously in the time of too much, and increases cost of manufacture.Be suitable generally to add 10 parts of edible ethanols.
The natural clarifying agent that the present invention adopts is the ZTC1+1 natural clarifying agent that Tianjin became the clarification technique company limited to produce in positive day, its role is to remove impurity such as macromolecular substances such as protein in the extracting solution, tannin, natural gum, makes solution be easy to filter.
The Herba Solani Lyrati extract of the present invention preparation very easily makes moist, soluble in water, dissolve in methanol, ethanol, sweet-bitter flavor, concentration be 1% water-solublely easily be brown.
The Herba Solani Lyrati extract of the present invention preparation be with thin layer chromatography to wherein solasodine, tomatidine and dioscin are analyzed, concrete steps are as follows:
Thin layer chromatography
Test solution: below 50~80 ℃, the ethanol extraction (about 1: 4.5) of vacuum evaporation Herba Solani Lyrati (Solanum Lyratum Thumb) stem is to dry.
The about 0.20g of extract adds 20~30ml methanol and a small amount of dense HCL back hydrolysis 13 hours in flask, reclaim methanol then and remain 10~15ml to bottle end approximately, take out bottle, put coldly, add distilled water and 10~20ml strong aqua ammonia (35%) and change over to and uses methylbenzene extraction in the separatory funnel, toluene layer filters with absorbent cotton, water layer continues to use methylbenzene extraction secondary, combining methylbenzene liquid, reclaim under reduced pressure, remove most toluene, residue is with 1~10ml dissolve with methanol.
Contrast liquid: solasodine (Solasodine), tomatidine (Tomatidine) and each about 2mg of dioscin (Diosgenin) are dissolved in respectively among 1~10ml methanol R.
Adsorbent: gel GF 254 plate.At 110 ℃ of oven dry 30~60min, put in the exsiccator and treat coldly usefulness after the gel GF 254 plate system.
Developing solvent: (chloroform, water, methanol proper proportion) takes off layer.
The little bands of a spectrum of point sample: 12mm: 6 μ l test solutions (30mg ethanol extraction), 2 μ l dioscin liquid (=2 μ l dioscin liquid) and 4 μ l solasodines and Fructus Lycopersici esculenti alkali liquor (2 μ l reference substance).
Measure: air-dry chromatosheet (plate 1), use about 5ml developer: (vanillin, sulphuric acid, ethanol proper proportion) sprays onboard, high temperature (reaching 100~110 ℃) hot plate 5~7 minutes, clear to developing the color (plate 2).
Estimate: inspect under ultraviolet light (UV), 3~4 blue bands of a spectrum are arranged at the chromatogram bottom, and wherein 2 is solasodine reference substance and tomatidine.Another blue bands of a spectrum are much of light color between solasodine reference substance and tomatidine reference substance.Olive colour bands of a spectrum are arranged directly over tomatidine.On chromatogram top an olive colour extremely yellow chromatographic band is arranged, belong to dioscin.Be indigo plant-purple bands of a spectrum directly over it, a purple chromatographic band (plate 3) arranged near the edge.
The Herba Solani Lyrati extract that the present invention obtained, its effective active position mainly is that steroid alkaloid has effects such as antiinflammatory, can be made into the ointment of treatment eczema and dermatomycosis after the adding different auxiliary material.Owing to Herba Solani Lyrati extract belongs to the pure natural medical preparation, hormone-like effect is arranged, but do not have the untoward reaction behind the use hormone, it has a extensive future.
Fairly simple, the easy enforcement of Herba Solani Lyrati extract preparation method, product recovery rate that the present invention adopts are bigger.
The specific embodiment
Embodiment 1:
Buy 10 kilograms of Herba Solani Lyrati medical materials, through pulverizing, cross 40 mesh sieves, soaked 1 hour with 100 kilogram of 30% edible ethanol, be heated to about 70 ℃ and be incubated 70 minutes, emit while hot and filter, time soak of winning the first place, be 30% edible ethanol toward 50 kilograms of medicinal residues addings and 30 kilograms of concentration at twice successively then, be heated to about 70 ℃ equally respectively and be incubated 60 minutes, emit while hot and filter, win the second place time and soak for the third time, three soaks are combined, with the decompression decompression recycling ethanol, and be concentrated into about 50 kilograms, add powdered activated carbon 100 grams, stir, put cold.Under fully stirring, add clarifier (two kinds of each 100 grams of A, B), left standstill 18 hours, make abundant precipitation, cross elimination precipitation, reuse 800 gram clear water are washed precipitation, all are soaked clear liquids concentrate and be dried to solid under vacuum condition, the plastic bag of packing into, extract and medical material were than about 1: 10.
Embodiment 2:
Buy 11 kilograms of Herba Solani Lyrati medical materials, through pulverizing, cross 40 mesh sieves, soaked 1 hour with 140 kilogram of 30% edible ethanol, be heated to about 65 ℃ and be incubated 40 minutes, emit while hot and filter, time soak of winning the first place, be 30% edible ethanol toward 33 kilograms of medicinal residues addings and 33 kilograms of concentration at twice successively then, be heated to about 70 ℃ equally respectively and be incubated 50 minutes, emit while hot and filter, win the second place time and soak for the third time, three soaks are combined, with the decompression decompression recycling ethanol, and be concentrated into about 55 kilograms, add powdered activated carbon 120 grams, stir, put cold.Under fully stirring, add clarifier (two kinds of each 100 grams of A, B), left standstill 20 hours, make abundant precipitation, cross elimination precipitation, reuse 1000 gram clear water are washed precipitation, all are soaked clear liquids concentrate and be dried to solid under vacuum condition, the plastic bag of packing into, extract and medical material were than about 1: 9.
Embodiment 3:
Buy 9 kilograms of Herba Solani Lyrati medical materials, through pulverizing, cross 40 mesh sieves, soaked 1 hour with 72 kilogram of 30% edible ethanol, be heated to about 80 ℃ and be incubated 70 minutes, emit while hot and filter, time soak of winning the first place, be 30% edible ethanol toward 54 kilograms of medicinal residues addings and 45 kilograms of concentration at twice successively then, be heated to about 60 ℃ equally respectively and be incubated 70 minutes, emit while hot and filter, win the second place time and soak for the third time, three soaks are combined, with the decompression decompression recycling ethanol, and be concentrated into about 45 kilograms, add powdered activated carbon 120 grams, stir, put cold.Under fully stirring, add clarifier (two kinds of each 100 grams of A, B), left standstill 24 hours, make abundant precipitation, cross elimination precipitation, reuse 1000 gram clear water are washed precipitation, all are soaked clear liquids concentrate and be dried to solid under vacuum condition, the plastic bag of packing into, extract and medical material were than about 1: 9.
Claims (3)
1. the preparation method of a plant of Solanaceae Herba Solani Lyrati extract is characterized in that this method comprises the step (umber of admixture is a weight portion) of following order:
(1) with 1 part of Herba Solani Lyrati pulverizing medicinal materials, add 8~13 parts of edible ethanols and soak post-heating to 60~85 ℃ insulation in 0.8~1.2 hour 40~70 minutes, filtered while hot is emitted soak for the first time subsequently, then add 4~7 parts of edible ethanols and be heated to 60~85 ℃ of insulations 40~70 minutes toward medicinal residues, filtered while hot goes out soak for the second time, and last past again medicinal residues add 3~6 parts of edible ethanols and obtain soak for the third time with same heating-up temperature and temperature retention time;
(2) three soaks that step (1) is obtained combine, and adopt the decompression method to reclaim ethanol, and soak is concentrated into 4~6 parts;
(3) under well-beaten situation, add two kinds each 0.01~0.012 part of natural clarifying agent A and B, leave standstill and be no less than 10 hours and allow soak fully precipitate, remove by filter precipitation then, add again and be not more than 0.1 part of clear water washing precipitation, filtering the back adds in the soak, the immersion clear liquid that is obtained adopts the decompression method to concentrate, and is dried to the blocks of solid extract under vacuum condition.
2. the preparation method of Herba Solani Lyrati extract according to claim 1 is characterized in that described edible ethanol is the edible ethanol of 30% concentration.
3. the preparation method of Herba Solani Lyrati extract according to claim 1 is characterized in that after the Herba Solani Lyrati concentrated solution that step (2) obtains, also add put after 0.01~0.012 part of active carbon stirs cold.
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CN 200410051623 CN1634295A (en) | 2004-09-27 | 2004-09-27 | Preparation method for climbing nightshade extract |
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CN 200410051623 CN1634295A (en) | 2004-09-27 | 2004-09-27 | Preparation method for climbing nightshade extract |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102093345A (en) * | 2010-12-21 | 2011-06-15 | 浙江工业大学 | Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography |
CN102319319A (en) * | 2011-09-15 | 2012-01-18 | 中国中医科学院西苑医院 | Solanum lyratum extract, and anticancer medicine comprising solanum lyratum extract |
CN104020227A (en) * | 2014-05-21 | 2014-09-03 | 浙江理工大学 | Alkali content determination method for steroid alkaloid produced by tissue culture method |
CN106928309A (en) * | 2017-02-17 | 2017-07-07 | 中国中医科学院西苑医院 | A kind of spirosolane type glycoalkaloid and preparation method thereof and purposes |
CN106939031A (en) * | 2017-02-17 | 2017-07-11 | 中国中医科学院西苑医院 | A kind of spirosolane type glycoalkaloid and preparation method thereof and purposes |
-
2004
- 2004-09-27 CN CN 200410051623 patent/CN1634295A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102093345A (en) * | 2010-12-21 | 2011-06-15 | 浙江工业大学 | Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography |
CN102093345B (en) * | 2010-12-21 | 2013-03-27 | 浙江工业大学 | Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography |
CN102319319A (en) * | 2011-09-15 | 2012-01-18 | 中国中医科学院西苑医院 | Solanum lyratum extract, and anticancer medicine comprising solanum lyratum extract |
CN102319319B (en) * | 2011-09-15 | 2013-05-08 | 中国中医科学院西苑医院 | Solanum lyratum extract, and anticancer medicine comprising solanum lyratum extract |
CN104020227A (en) * | 2014-05-21 | 2014-09-03 | 浙江理工大学 | Alkali content determination method for steroid alkaloid produced by tissue culture method |
CN104020227B (en) * | 2014-05-21 | 2015-08-19 | 浙江理工大学 | A kind of tissue culture method produces the alkali content assay method of steroid alkaloid |
CN106928309A (en) * | 2017-02-17 | 2017-07-07 | 中国中医科学院西苑医院 | A kind of spirosolane type glycoalkaloid and preparation method thereof and purposes |
CN106939031A (en) * | 2017-02-17 | 2017-07-11 | 中国中医科学院西苑医院 | A kind of spirosolane type glycoalkaloid and preparation method thereof and purposes |
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