CN102579543B - Method for extracting Traditional Chinese medicine active ingredients of marigold inflorescences - Google Patents
Method for extracting Traditional Chinese medicine active ingredients of marigold inflorescences Download PDFInfo
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- CN102579543B CN102579543B CN 201210072716 CN201210072716A CN102579543B CN 102579543 B CN102579543 B CN 102579543B CN 201210072716 CN201210072716 CN 201210072716 CN 201210072716 A CN201210072716 A CN 201210072716A CN 102579543 B CN102579543 B CN 102579543B
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- flos tagetis
- tagetis erectae
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Abstract
The invention relates to a method for extracting Chinese medicinal active ingredients of marigold inflorescences, and belongs to the technical field of the preparation of active ingredients of Chinese herbal medicines. The method comprises the following steps of: extracting the marigold inflorescences which are dried, are not mildewed, and do not have impurities and other wastes by water-alcohol mixed liquid, after alcohol is removed, removing unsaturated fatty acid by using a calcium agent, and concentrating and drying to obtain the Chinese medicinal active ingredients of the marigold inflorescences, which do not contain protein and can be dissolved in water. The Chinese medicinal active ingredients of the marigold inflorescences, which are extracted by the technology, do not contain the protein, particularly the unsaturated fatty acid, various Chinese medicinal active ingredients of the original medicinal materials are reserved, and mildew and oxidation rancidity are avoided during storage, so that great convenience is brought to the use of Chinese medicines in preparation and health-care food.
Description
Technical field
The present invention relates to a kind of Chinese herbal medicine technology of preparing, particularly relate to inflorescence class Chinese crude drug active ingredient preparation method, belong to effective component of Chinese herbal medicine preparation technique field.
Technical background
Flos Tagetis Erectae, annual herb, in the Flos Tagetis Erectae inflorescence, containing phylloxanthin and lutein ester, this is that current many people are as the important materials of producing phylloxanthin.Extract in Flos Tagetis Erectae flavochrome oil component and contain the multiple fatty acids such as lauric acid, myristic acid, Palmic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, arachidic acid.
The patented technology of now many relevant Flos Tagetis Erectaes, except cultivation technique, be all to extract phylloxanthin, and the process technology that the Flos Tagetis Erectae inflorescence is used as Chinese crude drug has no report.
The inflorescence of plant Flos Tagetis Erectae shines dry-storage, is medical material Ji Yuan.The Flos Tagetis Erectae inflorescence contains patuletin, quercetagetin, ten thousand is helped echinacoside, quercetagitrin, α-tri-thiophene, Z-ocimenone, E-ocimenone, limonene, β Flos Caryophylli alkene, tagetone, piperitone and Mentha piperita ketenes, and this is the pharmacological basis of Flos Tagetis Erectae inflorescence as the Chinese herbal medicine medical material.
" China book on Chinese herbal medicine ": be used for the treatment of the diseases such as upper respiratory tract infection, pertussis, conjunctivitis, stomatitis, toothache, pharyngitis, dizzy, infantile convulsion, amenorrhea, abdominal pain due to blood stasis, carbuncle pyogenic infections from tumour or sore, anti-dispelling the wind and dampness pathogens.
Medicinal raw material Flos Tagetis Erectae inflorescence dries and uses when the Chinese medicine dispensing as medical material afterwards.The inflorescence dried safety in storage can not be guaranteed.The Flos Tagetis Erectae inflorescence dried comes from the Nature, inevitably has antibacterial, mycete, insecticide worm's ovum etc., duration of storage, and the impact of temperature, the impact of humidity, these biologies are growth and breeding probably, very harmful to health.Particularly mycete exists, and the mycotoxin of generation is the carcinogenic factor.In addition, in the Flos Tagetis Erectae inflorescence dried, owing to containing the unsaturated fatty acids such as oleic acid, linoleic acid, be easy to oxidative rancidity, produce small molecule aldehyde material, harmful.
The present invention is based on such understanding, from the Flos Tagetis Erectae inflorescence, above-mentioned active ingredient is separated, as medicinal raw material and the healthy food material of preparation Chinese patent medicine.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of from the Flos Tagetis Erectae inflorescence, above-mentioned active ingredient being separated, and this effective components of Chinese medicinal can be as medicinal raw material and the healthy food material of preparation Chinese patent medicine.
For solving the problems of the technologies described above, technical scheme of the present invention is achieved in that a kind of method of extracting Chinese medicinal active ingredients of marigold inflorescences, it is characterized in that: use is dry, nothing is gone mouldy, the Flos Tagetis Erectae inflorescence of no-sundries; By the extraction of ethanol-water mixed liquor, make Flos Tagetis Erectae inflorescence slag and the solution that contains Flos Tagetis Erectae inflorescence solvent components carry out solid-liquid separation; After removing wherein ethanol, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence; Remove the unsaturated fatty acid in aqueous solution with calcium preparation again; Finally, concentrate drying obtains the Flos Tagetis Erectae inflorescence not containing protein and water-soluble effective components of Chinese medicinal.
Use is dry, nothing is gone mouldy, the Flos Tagetis Erectae inflorescence of no-sundries, and its moisture content is between 10～45%.
Described ethanol-water mixed liquor extraction, make the percentage by weight of water, ethanol in Flos Tagetis Erectae inflorescence solvent components be, the ratio of water is 20～50%, and the ethanol ratio is 50～80%.
The Flos Tagetis Erectae inflorescence of described drying dries, or is not having to dry under sunlight, or oven drying at low temperature.
Described solid-liquid separation is to use the filter press method, or adopts centrifugal separation method.
Described centrifugalize can be link-suspended basket centrifuge, vertical centrifugal machine, disc centrifuge.
Described calcium preparation is saturated aqua calcis, and its consumption is 10～20% of aqueous solution weight.
Described calcium preparation is saturated calcium carbonate soln, and its consumption is 20～30% of aqueous solution weight.
Described calcium preparation is granular calcium hydroxide, and its consumption is 2～4% of aqueous solution weight.
Described calcium preparation is granular calcium carbonate, and its consumption is 3～6% of aqueous solution weight.
Described finally dried mode adopts spray drying, or lyophilisation, or non-lyophilisation.
Described its mode of non-lyophilisation comprises: the drying of bipyramid rotary vacuum drying, rake vacuum drying, three kinds of forms of board-like vacuum drying.
Beneficial effect of the present invention, the present invention obtains the inflorescence effective components of Chinese medicinal by soaking extracting process, not containing protein, especially not containing unsaturated fatty acid, and retained various original medical material effective components of Chinese medicinal, obtain can be used as preparing the pure medicinal raw material of Chinese crude drug after drying.At duration of storage, be not easy to go mouldy, more can not oxidative rancidity.And be very easy to while using Chinese medicine dispensing and use and the health food use.
The present invention can be extracted Effective Component of Chinese Medicine, and the application of technology, to the technology innovation of Chinese medicine manufacturing enterprise, increases enterprise competitiveness, promotes the raising of Chinese Medicine Industry comprehensive benefit to have positive effect.
The specific embodiment
Embodiment 1
In embodiment, material is used by weight percentage.
Choose a certain amount of pollution-free, without disease and pest, without the Flos Tagetis Erectae inflorescence of various foreign material and rubbish, these Flos Tagetis Erectae inflorescences are dried, also can ventilate in the cool and dry or dry with equipment under the sun, make its moisture content between 10～45%; Then process as follows:
A. first determine moisture content;
B. according to the moisture content in A, in dry Flos Tagetis Erectae inflorescence material, throwing in is in the ethanol-water mixed liquor of 3～5 times of solid contents, makes the water in Flos Tagetis Erectae inflorescence solvent components: ethanol=0.5: 0.5;
C. the solid content of moisture-ethanol with the plate type pressure filter filtrate of squeezing out, Flos Tagetis Erectae inflorescence slag and the solution that contains Flos Tagetis Erectae inflorescence solvent components are carried out to solid-liquid separation.
D. filtrate is carried out to water and separate with ethanol, with the alcohol distillation tower, isolate ethanol, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence, the ethanol recycling;
E. by containing the water-soluble liquid measure of the various solvable compositions of Flos Tagetis Erectae inflorescence the number, add 10～20% saturated aqua calcises of water-soluble liquid measure in filtrate, quiescent setting, obtain supernatant;
F. the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence of disgorging is carried out to low temperature, concentrating under reduced pressure, obtain containing the aqueous solution that the various solvable compositions of Flos Tagetis Erectae inflorescence are 20～30%;
The aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence that G. will concentrate with spray dryer carries out spray drying, obtains the water solublity active ingredient extract of Flos Tagetis Erectae inflorescence, is pulverulence finished product thing.
Embodiment 2
In embodiment, material is used by weight percentage
Choose a certain amount of pollution-free, without disease and pest, without the Flos Tagetis Erectae inflorescence of various foreign material and rubbish, these Flos Tagetis Erectae inflorescences are dried, also can ventilate in the cool and dry or dry with equipment under the sun, make moisture content between 10～45%; Then process as follows:
A. determine moisture content;
B. according to the moisture content in A, in dry Flos Tagetis Erectae inflorescence material, throwing in is the ethanol-water mixture liquid of 3～5 times of solid contents, soaks.Make the water in Flos Tagetis Erectae inflorescence solvent components: ethanol=0.4: 0.6.
C. carry out solid-liquid separation with link-suspended basket centrifuge, obtain the coarse filtration liquid that contains a small amount of molecule;
D. above-mentioned thick liquid is filtered with vertical centrifugal machine again, obtains not having the filtrate of impurity;
E. isolate ethanol with the alcohol distillation tower, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence, the ethanol recycling;
F. by containing the water-soluble liquid measure of the various solvable compositions of Flos Tagetis Erectae inflorescence the number, add 20～30% saturated calcium carbonate solns of water-soluble liquid measure in filtrate, quiescent setting, obtain supernatant;
G. the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence of disgorging is carried out to low temperature, concentrating under reduced pressure, obtain containing the aqueous solution that the various solvable compositions of Flos Tagetis Erectae inflorescence are 40～50%;
The aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence that H. will concentrate with freeze drying equipment carries out lyophilization, obtains the water solublity active ingredient extract of Flos Tagetis Erectae inflorescence.
I. dried crushing material is obtained to pulverulence finished product thing.
Embodiment 3
In embodiment, material is used by weight percentage
Choose a certain amount of pollution-free, without disease and pest, without the Flos Tagetis Erectae inflorescence of various foreign material and rubbish, these Flos Tagetis Erectae inflorescences are dried, also can ventilate in the cool and dry or dry with equipment under the sun, make moisture content between 10～45%; Then process as follows:
A. determine moisture content;
B. according to the moisture content in A, in dry Flos Tagetis Erectae inflorescence material, throwing in is the ethanol-water mixed liquor of 3～5 times of solid contents, soaks.Thereby make the water in Flos Tagetis Erectae inflorescence solvent components: ethanol=0.2: 0.8.
C. carry out solid-liquid separation with the continuous solid-liquid separating machine machine, obtain the coarse filtration liquid that contains a small amount of molecule;
D. above-mentioned thick liquid is filtered with disc centrifuge again, obtains not having the filtrate of impurity;
E. isolate ethanol with the alcohol distillation tower, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence, the ethanol recycling;
F. by containing the water-soluble liquid measure of the various solvable compositions of Flos Tagetis Erectae inflorescence the number, add the granule of 2～4% calcium hydroxide of water-soluble liquid measure in filtrate, stir 15～30 minutes, quiescent setting, obtain supernatant;
G. the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence of disgorging is carried out to low temperature, concentrating under reduced pressure, obtain containing the aqueous solution that the various solvable compositions of Flos Tagetis Erectae inflorescence are 40～50%;
The aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence that H. will concentrate with vacuum dryer carries out vacuum drying, obtains the water solublity active ingredient extract of Flos Tagetis Erectae inflorescence;
I. dried crushing material is obtained to pulverulence finished product thing.
Embodiment 4
In embodiment, material is used by weight percentage
Choose a certain amount of pollution-free, without disease and pest, without the Flos Tagetis Erectae inflorescence of various foreign material and rubbish, these Flos Tagetis Erectae inflorescences are dried, also can ventilate in the cool and dry or dry with equipment under the sun, make moisture content between 10～45%; Then process as follows:
A. determine moisture content;
B. according to the moisture content in A, with Chinese medicine Continuous Countercurrent Extraction equipment, in dry Flos Tagetis Erectae inflorescence material, throwing in is the ethanol-water mixture of 3～5 times of solid contents, soaks.Make the water in Flos Tagetis Erectae inflorescence solvent components: ethanol=0.45: 0.55.
C. carry out solid-liquid separation with continuous solid-liquid separating machine, obtain the coarse filtration liquid that contains a small amount of molecule;
D. above-mentioned coarse filtration liquid is filtered with butterfly chip centrifuge again, obtains not having the filtrate of impurity;
E. isolate ethanol with the alcohol distillation tower, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence, the ethanol recycling;
F. the subsider that uses Chinese traditional medicine machine factory to provide, by containing the water-soluble liquid measure of the various solvable compositions of Flos Tagetis Erectae inflorescence the number, in filtrate, adding is 3～6% calcium carbonate superfine powders of water-soluble liquid measure, precipitation obtains supernatant;
G. the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence of disgorging is carried out to low temperature, concentrating under reduced pressure, obtain containing the aqueous solution that the various solvable compositions of Flos Tagetis Erectae inflorescence are 40～50%;
The aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence that H. will concentrate with hot air drying equipment carries out drying, obtains the water solublity active ingredient extract of Flos Tagetis Erectae inflorescence;
I. dried crushing material is obtained to pulverulence finished product thing.
Above-mentioned solid-liquid separation can be used the filter press method, also can adopt centrifugal separation method.And three kinds of centrifugalize can be link-suspended basket centrifuge, vertical centrifugal machine, disc centrifuge.During the solid-liquid separation operation, can be used in conjunction with.
Above-mentioned finally dried mode can adopt spray drying, or lyophilisation, or non-lyophilisation.But not its mode of lyophilisation can be bipyramid rotary vacuum drying or rake vacuum drying or board-like vacuum-dried form.
The description of the above-mentioned embodiment of the present invention, be the specific embodiment of the invention, but can not limit protection scope of the present invention with this, and variation and the modification in every case done in this way, all within protection scope of the present invention.
Claims (5)
1. a method of extracting Chinese medicinal active ingredients of marigold inflorescences is characterized in that: use dry, without going mouldy, the Flos Tagetis Erectae inflorescence of no-sundries; By the extraction of ethanol-water mixed liquor, make Flos Tagetis Erectae inflorescence slag and the solution that contains Flos Tagetis Erectae inflorescence solvent components carry out solid-liquid separation; After removing wherein ethanol, obtain the aqueous solution containing the various solvable compositions of Flos Tagetis Erectae inflorescence; Remove the unsaturated fatty acid in aqueous solution with calcium preparation again; Finally, concentrate drying obtains the Flos Tagetis Erectae inflorescence containing protein and water-soluble effective components of Chinese medicinal, and in described ethanol-water mixed liquor extraction, water, ethanol percentage by weight be, the ratio of water is 20～50%, and the ethanol ratio is 50～80%; Described calcium preparation is saturated aqua calcis, its consumption is 10～20% of aqueous solution weight, perhaps calcium preparation is saturated calcium carbonate soln, its consumption is 20～30% of aqueous solution weight, perhaps calcium preparation is granular calcium hydroxide, its consumption is 2～4% of aqueous solution weight, or calcium preparation is granular calcium carbonate, and its consumption is 3～6% of aqueous solution weight.
2. a kind of method of extracting Chinese medicinal active ingredients of marigold inflorescences according to claim 1 is characterized in that: described use dry, without going mouldy, the Flos Tagetis Erectae inflorescence of no-sundries, its moisture content is between 10～45%.
3. a kind of method of extracting Chinese medicinal active ingredients of marigold inflorescences according to claim 1, it is characterized in that: the Flos Tagetis Erectae inflorescence of described drying dries, or is not having to dry under sunlight, or oven drying at low temperature.
4. a kind of method of extracting Chinese medicinal active ingredients of marigold inflorescences according to claim 1 is characterized in that: described solid-liquid separation is to use the filter press method, or adopts centrifugal separation method.
5. according to a kind of described method of extracting Chinese medicinal active ingredients of marigold inflorescences of any one in claim 1 to 4, it is characterized in that: described finally dried mode adopts spray drying, or lyophilisation, or non-lyophilisation.
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Granted publication date: 20131218 Termination date: 20170316 |