Patent File 229 Marigold extract
ในดาวเรือง (Tagetes erecta) ที่มีสีเหลืองส้มมีสารที่มีประโยชน์ เช่น แคโรทีนอยด์ เฟลโวนอยด์ ซึ่งสามารถนำไปประยุกต์ใช้กับผลิตภัณฑ์ต่าง ๆ ได้ ในเอกสารสิทธิบัตรมีข้อมูลความรู้เกี่ยวกับสารสกัดจาดาวเรื่อง วิธีสกัด ฯลฯ ตามตัวอย่างเอกสารสิทธิบัตรด้านล่าง
| No. | Patent Number | Title | Abstract |
| 1 | CN 105,693,675 | A method of extracting flavonoid compounds from tagetes erecta | A method of extracting flavonoid compounds from tagetes erecta is provided. The method includes a step of drying tagetes erecta dry flowers, grinding into powder, dipping with ethanol or performing reflux extraction, subjecting a filtrate after filtration to rotary evaporation until a product is dry and dissolving the product into a methanol-water mixed solvent; a step of performing one-dimensional liquid chromatographic analysis, wherein DAISO C18 is adopted as a chromatographic column, a mobile phase adopting water as an A phase and methanol as a B phase is adopted, isocratic elution is performed for 20 min with the concentration of the B phase in the mobile phase being 50-55%, eluate from the 11 min to the 14 min is collected according to an ultraviolet absorption spectrum, adopted as target components, and subjected to rotary evaporation until a product is dry, and the product of the rotary evaporation is dissolved into the methanol-water mixed solution again; and a step of performing two-dimensional liquid chromatographic analysis, wherein Acchrom X-Amide is adopted as a chromatographic column, a mobile phase adopting water as an A phase and acetonitrile as a B phase is adopted, isocratic elution is performed for 40 min with the concentration of the B phase in the mobile phase being 92-98%, and eluate from the 12 min to the 17 min is collected according to an ultraviolet absorption spectrum, adopted as the target components, and subjected to rotary evaporation until a product is dry to obtain the flavonoid compounds. |
| 2 | CN 105,693,676 | A method of separating and purifying quercetagetin from tagetes erecta | A method of separating and purifying quercetagetin from tagetes erecta is provided. The method includes a step of drying tagetes erecta dry flowers, grinding into powder, dipping with ethanol or performing reflux extraction, subjecting a filtrate after filtration to rotary evaporation until a product is dry and dissolving the product to a methanol-water mixed solvent; a step of performing one-dimensional liquid chromatogram, wherein DAISO C18 is adopted as a chromatographic column, a mobile phase adopting water as an A phase and methanol as a B phase is adopted, isocratic elution is performed for 20 min with the concentration of the B phase in the mobile phase being 50-55%, eluate from the 6 min to the 12 min is collected according to an ultraviolet absorption spectrum, adopted as a target component, and subjected to rotary evaporation until a product is dry, and the product of the rotary evaporation is dissolved into the methanol-water mixed solution again; and a step of performing two-dimensional liquid chromatogram, wherein Acchrom X-Amide is adopted as a chromatographic column, a mobile phase adopting water as an A phase and acetonitrile as a B phase is adopted, isocratic elution is performed for 40 min with the concentration of the B phase in the mobile phase being 92-98%, and eluate from the 27 min to the 33 min is collected according to an ultraviolet absorption spectrum, adopted as the target component, and subjected to rotary evaporation until a product is dry to obtain quercetagetin the purity of which is 99% or above. |
| 3 | US 6,086,885 | Anti-bacterial protein extracts from seeds of marigold and paprika | The present invention describes the method of extraction and the effect of a crude protein extract from the seed tissue of two botanical species, Tagetes and Capsicum, on the survival of two economically important gram-negative bacteria Salmonella typhimurium and Escherichia coli. |
| 4 | CN 104,086,038 | Comprehensive processing method for squeezing sewage generated in process of extracting xanthophyll from tagetes erecta | A disclosed comprehensive processing method for squeezing sewage generated in a process of extracting xanthophyll from tagetes erecta comprises the following steps: performing preliminary precipitation; filtering the upper-layer liquid, adding aerobic activated sludge into the filtrate and aerating for 8-10 days; performing precipitation on the aerated upper-layer liquid; adding anaerobic activated sludge into the upper-layer liquid subjected to precipitation and performing anaerobic fermentation for 8-20 days, and collecting generated biogas; performing precipitation on the supernatant subjected to anaerobic fermentation; filtering the upper-layer liquid subjected to precipitation, and performing decolouring processing; and enabling a clear liquid subjected to decolouring to flow out and storing in constructed wetland.; Through precipitation, filtering, aeration, anaerobic fermentation, decolouring and constructed-wetland storage for comprehensively processing squeezing sewage generated in the process of extracting xanthophyll from tagetes erecta, the comprehensive processing method is low in cost, reasonable in economy and small in consumption, is capable of substantially reducing COD of squeezing sewage and purifying water quality, obtaining biogas energy source, and finally enabling wastewater to reach the standard by combining constructed-wetland ecological processing, helps to beautify environment, is high in automation degree and helps to reduce labor intensity. |
| 5 | WO 9,826,671 | Extract and Formulation for the Pigmentation of Chicken Skin and the Yolk, and Process for Its Administration | The invention relates to a saponified extract of Tagetes Erecta L.(cempasuchil) of which the zeaxanthin content is comprised between 20 % and 80 % of the total of xantophyles, as well as a formulation and a process for its dosing, comprising and administering approximately between 10 and 55 ppm of the saponified xantophyles of cempasuchil which have a zeaxanthine content comprised between 20 and 80 % to the food or beverage of birds in order to provide for the skin pigmentation of chicken and the pigmentation of the yolk and give them the commercially required coloration. |
| 6 | US 7,622,599 | Isolation and purification of carotenoids from marigold flowers | The present invention explains a realistic and effective process for isolating and purifying carotenoids containing higher concentrations of carotenoids such as trans-lutein, trans-zeaxanthin, Cis-lutein, .beta.-carotene and Cryptoxanthin from Marigold flower petals under controlled conditions leaving no traces of any organic hazardous solvents. The process involves ensilaging Marigold flowers, dehydration, solvent extraction, alkali hydrolysis of carotenoid esters with absolute alcohol, crystallization/purification using water, absolute alcohol mixture followed by filteration and drying until the crystals are considerably free from moisture and absolutely free from residual hazardous solvents. These crystals are suitable for nutraceutical and food products as supplements. |
| 7 | US 8,481,769 | Isolation and purification of cartenoids from marigold flowers | A process for isolation of carotenoids crystals having lutein and zeaxanthin in a weight ratio of about 10:1, 5:1 or 1:1. The process comprises contacting a plant source rich in lutein with hexane and extracting at a temperature of about 40.degree. C. to 60.degree. C. to obtain an oleoresin rich in lutein; contacting a plant source rich in zeaxanthin with hexane and extracting at a temperature of about 40.degree. C. to 60.degree. C. to obtain an oleoresin rich in zeaxanthin. The oleoresin rich in lutein and the oleoresin rich in zeaxanthin are mixed separately in a ratios ranging from about 80:20 (w/w) to 90:10 (w/w) or about 70:30 (w/w) to 30:70 (w/w) or about 10:90 (w/w) to 20:80 (w/w) and homogenized to obtain a mixed oleoresin. The mixed oleoresin is hydrolyzed with an alcoholic alkali at a temperature of about 70.degree. C. to 80.degree. C. to obtain a reaction mixture. The carotenoids crystals are precipitated by adding hot water to the reaction mixture to form a precipitate. Carotenoids crystals having lutein and zeaxanthin in a ratio of about 10:1 or 5:1 or 1:1 respectively are obtained by filtering, washing and drying the precipitate. |
| 8 | CN 1,120,565 | Method for extracting lutein resin edible pigment from Tagetes erecta flower | The process for extracting lutein resin as edible pigment from marigold flower includes fermenting collected marigold flower, drying, breaking, extracting with petroleum ether and heating extracted liquid for vaporization to obtain semi-finished product, cooling the vapour to obtain regenerated petroleum ether, deodouring said semi-finished product, removing residual petroleum ether by alcohol, and partially saponifying by potassium hydroxide. Obtained product has high purity and pure and stable hue. The extracted residue is used as additive for feed. |
| 9 | CN 105,601,601 | Method for extraction of 6-hydroxy kaempferol monomer compound from Tagetes erecta | The invention provides a method for extraction of a 6-hydroxy kaempferol monomer compound from Tagetes erecta. The method includes: taking Tagetes erecta dried flower, grinding the Tagetes erecta into powder, then subjecting the powder to ethanol soaking or reflux extraction, evaporating the filtrate to dryness, and then dissolving the extract in a methanol-water solvent; conducting one-dimensional liquid chromatography separation: employing a DAISO C18 chromatographic column and a water-methanol binary mobile phase, conducting isocratic elution with phase B at a concentration of 50-55%, collecting the 13-18min eluent, performing evaporation concentration to dryness; then dissolving the component in a methanol-water solvent; conducting two-dimensional liquid chromatography separation: employing an Acchrom X-Amide chromatographic column and a water-acetonitrile binary mobile phase, conducting isocratic elution with phase B at a concentration of 80-90%, collecting the 8-10min eluent, and carrying out evaporation concentration to dryness so as to obtain a target product. The method provided by the invention separates 6-hydroxy kaempferol from Tagetes erecta for the first time, and can reach purity up to more than 98%, thus providing more accurate guiding basis for quality control of Tagetes erecta and its preparations and rational clinical use of drugs. |
| 10 | CN 102,816,098 | Method for extraction of zeaxanthin from Tagetes erecta L. | Belonging to the technical field of extraction and separation of plant effective components, the invention provides a method for obtaining a Tagetes erecta L. extract with a zeaxanthin content of over 10% by supercritical CO2 extraction, macroporous resin chromatography and purification. In the process of extracting zeaxanthin from Tagetes erecta L. by a supercritical CO2 extraction method, no synthetic matter is introduced, and the pigment naturalness is kept. CO2 belongs to an inert gas, and is characterized by no toxicity, harmlessness, no residual, and no pollution on the raw material and the product. The method utilizes the modern technology of macroporous adsorption resin chromatography and purification to extract zeaxanthin from natural Tagetes erecta L., and after further separation, the purity of the zeaxanthin can reach 10%.; The invention adopts a novel solvent method to conduct separation and purification, avoids the use of toxic reagents, reduces solvent residual, guarantees the product quality, and improves the product recovery rate, thus bringing substantial convenience to industrialized production. |
| 11 | CN 102,838,519 | Method for separating and purifying all-trans high-purity lutein esters powder | The invention discloses a method for separating and purifying all-trans lutein esters powder prepared by Tagetes erecta granules, comprising the steps of mixing the Tagetes erecta granules and nonpolar solvent to perform continuously countercurrent supersonic extraction to obtain extract liquid, concentrating the extract liquid to obtain crude extract liquid extracts, dissolving the crude extract liquid extracts by solvent and using alumina column to perform column chromatography to obtain the high-purity lutein esters products.; According to the invention, the continuously countercurrent supersonic extraction is adopted to extract lutein esters, and the method has large batch processing capacity, less solvent using amount and high recovery rate, can reduce labor and power expenses, solves the technical problem that the lutein esters are directly purified from crude Tagetes erecta extracts by adopting the alumina column to perform chromatography of the lutein esters, and can prepare the all-trans lutein esters products with content more than 95% (HPLC: High Performance Liquid Chromatography), wherein the total carotenoid yield is more than 80 percent. |
| 12 | US 7,214,379 | Method for the purification of marigold oleoresin | Marigold oleoresin having a low viscosity and a high lutein content which can be filled in soft capsules can be obtained according to the method of the present invention, which is characterized by combining a step of subjecting oleoresin to supercritical fluid extraction and a step of dissolving oleoresin in a ketone solvent, cooling the solution and removing the ingredient which precipitated in solution. |
| 13 | US 9,012,698 | Method of extracting lutein/xanthophylls from natural materials and highly purified lutein/xanthophylls obtained from the method thereof | The present invention provides the new method for extracting lutein from natural materials wherein the said method comprises of modification of natural lutein ester in the natural materials to free lutein and/or low molecular weight lutein ester, extraction of the said natural materials with supercritical fluid at the optimal conditions. The said method yields high amount of crude lutein with high purity due to the mild condition used for extraction. Therefore, no degradation of the desired product is occurred. The crude lutein can be further purified with chromatography in order to obtain the highly purified lutein. The method according to this invention can be applied to the extraction of xanthophylls or others beside lutein. |
| 14 | CN 106,366,028 | New process for extracting high-content lutein ester from tagetes erecta l extract | The invention relates to a new process for extracting high-content lutein ester from a tagetes erecta l extract. The new process comprises: placing a tagetes erecta l extract into a closed container, carrying out closed extraction with an organic solvent, precipitating, filtering, rinsing the filter cake by using an alcohol, and drying the rinsed precipitate under a negative pressure condition to obtain the lutein ester with the content of not less than 80%, wherein the total yield is not less than 70%. According to the present invention, with the new process, the high-content lutein ester can be effectively extracted from the tagetes erecta l extracts having different qualities, and the problem that the tagetes erecta l extracts having different qualities require different extraction processes is solved; and the process has the simple operations and is suitable for industrial mass production. |
| 15 | GB 2,311,009 | Pharmaceutical compositions containing extracts of Tagetes (Marigolds) | Pharmaceutical base preparations comprise extracts of Asteraceae Tagetes , erecta (African Marigold), patula (French Marigold) or signata (Dwarf Marigold) or minuta . Preferably the compositions also contain extracts of any or a combination of the following: Bennis perennis , Hypericum perforatum , Symphytum officinalis , Thuja occidentalis , Thuja plicata , Ruta graveolens , Rosmarinus officinalis or Calendula arvensis . The preparations are particularly intended for the treatment of fungal infections of the nails, skin lesions, or disorders of the bones or joints. |
| 16 | CN 103,588,690 | Process for extracting xanthophyll from Tagetes erecta | The invention relates to a process for extracting xanthophyll from Tagetes erecta, and aims to provide a process which is used for extracting the xanthophyll from the Tagetes erecta and is simple to operate and suitable for industrial application. The process for extracting the xanthophyll from the Tagetes erecta comprises steps as follows: the Tagetes erecta is smashed; petroleum ether is used for extracting the xanthophyll; an extracting solution is subjected to reduced pressure concentration, and a fluid extract is obtained; the fluid extract is saponified, a saponifiable matter is dissolved in an ethanol solution and then filtered, and a filter cake is washed with the ethanol solution and then subjected to vacuum drying; and after a dried matter is mixed with an antioxidant, dichloromethane is used for recrystallization, an obtained crystal is subjected to vacuum drying, and a product is obtained. The process for extracting the xanthophyll from the Tagetes erecta is simple and facilitates industrial production; and the content of xanthophyll in a xanthophyll crude product washed with the ethanol solution is above 80%, the xanthophyll yield is above 35%, the content of the xanthophyll in the finally prepared product is above 95%, and the total yield of the xanthophyll is higher than 25%. |
| 17 | CN 105,254,549 | Process for extracting zeaxanthin from tagetes erecta l | The invention relates to a process for extracting zeaxanthin from tagetes erecta l, provides a method for obtaining a tagetes erecta l extract having a zeaxanthin content of more than 10% through supercritical CO2 extraction and macroporous resin chromatography purification, and belongs to the technical field of plant active ingredient extraction and separation. According to the present invention, the zeaxanthin in the tagetes erecta l is extracted through the supercritical CO2 extraction method, any synthesis substances are not introduced during the process, and the nature property of the pigment is maintained; the CO2 belongs to the inert gas, and has characteristics of no toxicity, no harm, no residue, no raw material pollution, and no product pollution; the modern process macroporous adsorption resin chromatography purification is used to extract the zeaxanthin from the natural tagetes erecta l so as to further achieve the separation purity of 10%; and the novel solvent method is used to separate and purify, such that the use of the toxic reagent is avoided, the solvent residue is reduced, the product quality is ensured, the product recovery rate is improved, and the great convenience is provided for the production industrialization. |
| 18 | US 6,262,284 | Process for extraction and purification of lutein, zeaxanthin and rare carotenoids from marigold flowers and plants | A process for simultaneously extracting, saponifying, and isolating lutein and zeaxanthin, and a mixture of several rare carotenoids in high purity from plants without the use of harmful organic solvents. Lutein crystals containing 5% zeaxanthin were obtained from the dried petals of Marigold flowers Tagete erecla while zeaxanthin was isolated and purified from the berries of Lycium Chinese Mill (LCM berries). Similarly, this process has been employed to isolate and purify a mixture of lutein, beta-carotene, neoxanthin, violaxanthin, and lutein epoxide from green plants, preferably, kale, collard green, and spinach. These plants, to a lesser extent, also serve as a source of several rare carotenoids such as alpha-cryptoxanthin (Marigolds) and beta-cryptoxanthin (LCM berries). The purified carotenoids isolated by this process are free from impurities and serve as a safe source of nutritional supplement for human consumption as well as providing a suitable and effective color additive for human foods. |
| 19 | US 7,173,145 | Process for extraction and purification of lutein, zeaxanthin and rare carotenoids from marigold flowers and plants | A process for extracting and isolating carotenoid esters or carotenoids in high purity from plants without the use of harmful organic solvents. Zeaxanthin esters were isolated and purified from the berries of Lycium Chinese Mill (LCM berries). The esters isolated according to the invention contain substantially no isomerized double bonds. The purified carotenoid esters or carotenoids isolated by this process are free from impurities and serve as a safe source of nutritional supplement for human consumption as well as providing a suitable and effective color additive for human foods. |
| 20 | US 9,109,120 | Process for isolation and purification of carotenoids | The present invention discloses a novel saponification process for the isolation and purification of highly pure carotenoids from different carotenoid rich oleoresin derived from plants and microorganisms without the use of toxic chemicals and hazardous solvents. The hydrolysis is carried out by treating the carotenoid rich oleoresin with a novel mixture of a Fatty alcohol, alkali and a fatty acid without the use of any other solvents. Further the invention explains a process of stabilizing the carotenoids from getting degraded due to high temperature and exposure time during the saponification process. Further the invention discloses an economically viable process of isolating high pure carotenoids with higher yield. |
| 21 | US 5,382,714 | Process for isolation, purification, and recrystallization of lutein from saponified marigold oleoresin and uses thereof | A method of isolating, purifying and recrystallizing substantially pure lutein, preferably from saponified marigold oleoresin in its pure free form, apart from chemical impurities and other carotenoids. Lutein may be used as an analytical standard or in cancer prevention trials and as a safe and effective color additive for human food. |
| 22 | US 7,150,890 | Process for the purification of marigold xanthophylls | Description of a process to extract, saponify and purify lutein and zeaxantine contained in Marigold flowers free from any genetic manipulation, which have been harvested by hand and dried upon weather so that it neither contains epoxicarotenoids or cis-carotenoids. Fatty acids are removed as its metallic salts and carotenoids are recovered using a polar solvent. |
| 23 | US 8,008,532 | Processes and methods for extraction and purification of lutein from marigold esters | A process is disclosed for simultaneously extracting, saponifying, and isolating lutein without the use of harmful organic solvents. In one embodiment the method includes (a) dispersing Marigold oleoresin in an alkane hydrocarbon alkanol solution, (b) adding a potassium hydroxide to the Marigold oleoresin and alkane hydrocarbon alkanol solution to form a homogenous solution of Marigold oleoresin, (c) refluxing the homogeneous solution until ester hydrolysis of the Marigold oleoresin is completed, (d) cooling the homogeneous solution and allowing it to settle until lutein crystals are formed, and (e) washing the lutein crystals with methanol-hexane solution to separate and filter them from the solvents. |
| 24 | US 6,329,557 | Purification of xanthophylls from marigold extracts that contain high levels of chlorophylls | The present invention provides an industrial scale process for obtaining lutein and zeaxanthin concentrates of high purity from saponified marigold extracts that may have high levels of chlorophyll. |
| 25 | US 5,959,138 | Short chain diesters and process for making the same | A process to obtain a product having a high content of zeaxanthin, lutein or mixtures thereof, as short chain organic acid diesters of zeaxanthin, lutein or mixtures thereof, that can be used mainly for the pigmentation of broilers and egg yolks, as well as an intermediate in the cantaxanthin( beta , beta -Carotene-4,4'-dione) and astaxanthin(3,3'-Dihidroxy beta , beta -carotene,4,4'-dione) synthesis, by reacting extracts obtained from marigold (Tagetes Erecta L.), or plant extracts that contain lutein, zeaxanthin or mixtures thereof in any proportion, with acetic or propionic anhydride under controlled conditions of temperature and pressure. |
| 26 | CN 106,748,945 | Simplest water-alcohol method for extracting axanthophylls from tagetes erecta flowers | At home and abroad, according to most traditional and existing methods, toxic organic solvent is adopted for extracting and refining axanthophylls from tagetes erecta flowers. The preparared axanthophylls is harmful to persons and pollutes the environment, the axanthophylls is extracted from the tagetes erecta flowers through the simplest water-alcohol method is high in safety for the persons and environmentally friendly, and the method is quite simple. |
| 27 | US 9,290,433 | Single stage lutein ester extraction from tagetes species-marigold flower meal | A single stage straight forward process for extraction and isolation of lutein ester from the dried petals of marigold flowers Tagetes species using the carbondioxide as the supercritical fluid was developed. The pressure maintained for the extraction was up to 625 bar and at temperature up to 750 Centigrade. Lutein ester of high strength and purity up to 70% was achieved for the first time in single stage from the dried petals of marigold flowers-Tagetes species while enrichment of the lutein ester content up to 98% was achieved by crystallization of the lutein ester obtained from supercritical carbon dioxide extract (SCFE). The high strength and purified lutein ester isolated by supercritical fluid-single stage extraction process are free from saturated fat, oil, waxy impurities and serve as a safe source of nutritional supplement for human consumption and color additive for human foods. |
| 28 | US 3,997,679 | Stabilization of xanthophylls | The xanthophyll esters, that are normally recovered from plant sources such as the marigold plant, Tagetes erecta, are selectively saponified. The neutralized, selectively saponified material, when incorporated into an inert carrier, provides a stable xanthophyll product having a pH above about 8. Such products have improved stabilities as compared to the original esters or to fully saponified esters. |
| 29 | CN 106,615,464 | Tagetes erecta flower tea, and preparation method thereof | The xanthophyll content of tagetes erecta flower is as high as 1 to 1.5%; xanthophyll and beta-carotene are capable of protecting the eyesight of human; and protection of eyesight is important for people of all ages and both sexes. The invention discloses a tagetes erecta flower tea solid beverage prepared taking tagetes erecta flower and beta-carotene as the main ingredients. Frequent drinking of the tagetes erecta flower tea solid beverage is capable of protecting the eyesight of human preferably; and excellent social effect is achieved. |
