WO2020048049A1 - 一种从罗汉果中制备罗汉果甜味组合物的方法及其应用 - Google Patents

一种从罗汉果中制备罗汉果甜味组合物的方法及其应用 Download PDF

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WO2020048049A1
WO2020048049A1 PCT/CN2018/123224 CN2018123224W WO2020048049A1 WO 2020048049 A1 WO2020048049 A1 WO 2020048049A1 CN 2018123224 W CN2018123224 W CN 2018123224W WO 2020048049 A1 WO2020048049 A1 WO 2020048049A1
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mogroside
han guo
luo han
extraction
fruit
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PCT/CN2018/123224
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English (en)
French (fr)
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张宝堂
谭家忠
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湖南绿蔓生物科技股份有限公司
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Priority to EP18932609.3A priority Critical patent/EP3795579B1/en
Priority to US17/274,153 priority patent/US20210274822A1/en
Publication of WO2020048049A1 publication Critical patent/WO2020048049A1/zh

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
    • A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30—Artificial sweetening agents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23L19/00—Products from fruits or vegetables; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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    • A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
    • A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
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    • A23L5/51—Concentration
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    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23N—MACHINES OR APPARATUS FOR TREATING HARVESTED FRUIT, VEGETABLES OR FLOWER BULBS IN BULK, NOT OTHERWISE PROVIDED FOR; PEELING VEGETABLES OR FRUIT IN BULK; APPARATUS FOR PREPARING ANIMAL FEEDING- STUFFS
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    • A61K47/46—Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Definitions

  • the invention belongs to the technical field of extraction and separation of plant active ingredients, and more particularly, relates to a method for preparing a sweet-grossing composition of Luo Han Guo from Luo Han Guo, and also relates to a compound sweet taste containing the sweet-growing composition of Luo Han Guo obtained by the above method. preparation.
  • Luo Han Guo Siraitia grosvenorii Swingle C. Jeffrey (formerly known as Momordica grosvenorii), also known as light fruit clogs, is the fruit of a perennial vine of the Cucurbitaceae family. Dioecious, flowering in summer and bearing fruit in autumn. Mainly produced in Guilin, Guangxi, China, Yongzhou, Shaoyang, Huaihua, Guangdong, Guangdong, etc. Luo Han Guo has green peel, long beach fruit, winter melon fruit, La Jiang fruit, red pit fruit, tung tree fruit and other varieties.
  • Luo Han Guo seedless Luo Han Guo (triploid seedless Luo Han Guo, parthenocarpy seedless Luo Han Guo) has also been planted in planting areas.
  • Luo Han Guo is also one of the first batch of dual-use materials for medicine and food approved by the country. Its main effect is to nourish the lungs, relieve cough, and regenerate phlegm.
  • the main sweet-smelling ingredient in Luo Han Guo is a class of saponins that use cucurbitane triterpenes such as Luo Han Guo alcohol as aglycones.
  • sweet-scented mogrosides include 11-O-mogroside V, neo-mogroside, mogroside V, iso-mogroside V, sammonin I, mogroside VI, mogroside IVe, mogroside IVa, etc .; no taste or taste
  • the bitter ones are Mogroside III (including Mogroside III, Mogroside IIIa1, Mogroside IIIe, Mogroside IIIe, etc.), Mogroside II (including Mogroside IIe, Mogroside IIa, Mogroside IIa1, Mogroside IIe, Mogroside) IIb, 11-O-Mogroside IIe, etc.), total Mogroside I (including mogroside Ia1, mogroside Ie1, etc.), among these saponins, mogroside V has the highest content, and mogroside V has good stability and calories Almost zero, sweetness up
  • Publication No. CN101007042B describes a method for preparing a decolorized and debittered Luo Han Guo extract, which uses 14 times water to infuse and cook Luo Han Guo, and then the resin absorbs ethanol to desorb the product.
  • a method for extracting mogroside V with publication number CN103923152B fresh mogroside is used as a raw material, and the fresh mogroside is washed, crushed, saccharified, extracted, and then settled and centrifuged. The macroporous resin is adsorbed and separated. Multi-resin column group selection is used. Adsorb, and collect desorption liquid in different sections.
  • U.S. patent US6124442 provides a dry composition containing mogroside containing mogroside. The obtained liquid is mixed with a solution having oxidation value, and then precipitated to clarify the liquid macroporous resin. Then the resin is eluted with alcohol, and the desorbed liquid is concentrated. Dry to obtain a dried composition containing a triterpene glycoside.
  • U.S. Patent No. 20110021456 provides a method for preparing a light-colored sweet composition without bitter impurities derived from Luo Han Guo.
  • the method for preparing Luo Han Guo sweet juice provided in the US patent US2014044843A1 is first extracted and then clarified, and then the extract is purified by using an anion exchange resin and a cation exchange resin to obtain a pure taste sweet juice composition.
  • composition has an effect, and these processes will hinder the production of organic Luo Han Guo extract. Moreover, the content of mogroside III, mogroside IIe, mogroside Ia1, and the isomers of these components in the product obtained in such a process is still high, and these components have a bad taste.
  • a first object of the present invention is to provide a method for extracting a sweetness composition from Luo Han Guo.
  • the method includes the following steps:
  • Luo Han Guo Put mature Luo Han Guo and immature Luo Han Guo together at a weight ratio of 1: 4 ⁇ 1: 8, seal them at 25 ⁇ 38 °C for 2 ⁇ 4 days, and then place them in a ventilated environment for 1 ⁇ 4 days to obtain Luo Han Guo.
  • the raw material is obtained by squeezing the juice of the Luo Han Guo raw material to obtain juice and fruit residue, combining the juice and the extract after extracting the fruit residue with pure water, removing impurities, and concentrating and purifying.
  • the yellow fruit stalk indicates that the fruit age of Luo Han Guo (the growth time from fruit formation to fruit picking) exceeds 3 months. It meets the requirements for picking, but most of these picked Luo Han Guo are still green or the skin surface is only partially yellow.
  • the main sweet components in such fresh fruits are Luo Han Guo V, Luo Han Guo VI, 11-O -Mogroside V, isomogroside V, etc.
  • the present invention ripens the green Luo Han Guo through the ethylene produced by the mature Luo Han Guo.
  • the ripening method includes: a) The golden yellow Luo Han Guo and the Green Luo Han Guo are arranged in a cross-section according to the appropriate weight to ensure maturity.
  • the ethylene released by Luo Han Guo can fully contact with Qing Luo Han Guo.
  • the weight ratio of mature Luo Han Guo and Qing Luo Han Guo is 1: 4 ⁇ 1: 8.
  • the temperature is 25 to 38 ° C for 2 to 4 days.
  • b) place it in a well-ventilated environment and leave it at room temperature for 1 to 4 days. Under the condition of air, it can ensure that the skin surface is dry to prevent mold growth and that Luo Han Guo can fully aerobically breathe, which is beneficial to the biotransformation process of Luo Han Guo.
  • the ripening is carried out by a method of directly introducing ethylene gas.
  • the temperature is in the range of 25 to 38 ° C, and the ethylene concentration is in the range of 500 ppm to 1500 ppm.
  • the green, sour, astringent, and bitter tastes of fresh Luo Han Guo fruit are significantly improved, and the sweetness is significantly enhanced.
  • the content of bitter-grossing mogrosides and non-sweet mogrosides in fresh mangosteen fruit was significantly reduced.
  • the content of mogroside III and mogroside IIe can be reduced to less than 10% of the original level.
  • the content of mogroside V and 11-O-mogroside V in raw materials can be increased to about 180% of the original content.
  • the fresh Luo Han Guo fruit used in the present invention can be the sub-genus Lo Han Guo and the scaleless Lo Han Guo in the genus Luo Han Guo of the Cucurbitaceae Vietnamese melon family, and can also be polyploid Luo Han Guo and seedless Luo Han Guo.
  • the subgenus of Luo Han Guo includes Luo Han Guo Siraitia, Grosvenorii (Swingle), C. Jeffrey, and Lu Zet Zhang, mainly produced in Guangxi, Guizhou, southern Hunan, Guangdong, and Jiangxi. Produced in western Guangxi and southeastern Yunnan, it can also be found in northern Vietnam and Thailand.
  • the scale-free Luo Han Guo subgenus has scale-free Luo Han Guo Siraitia borneensis (Merr.) C. Jeffrey ex Lu Zet Zhang, produced in Guangdong, Yunnan (Xichou) and Thu (Medog), also in Thailand, Malaysia; scale-free Luo Han Guo (original Variants) Siraitia borneensis (Merr.) C. Jeffrey, Lu, et al. ZYZhang, Var. Borneensis; C. Jeffrey, Siraitia borneensis (Merr.) C. Jeffrey, Ex. LuZet, ZYZhang, Var.
  • Organic Luo Han Guo refers to strictly following organic production regulations during the cultivation and growth of Luo Han Guo. It is forbidden to use any chemically synthesized pesticides, fertilizers, growth regulators and other chemical substances, and genetic engineering and its products are prohibited. Instead, it follows the natural law of Luo Han Guo growth. Luo Han Guo, which is based on ecological principles, has been certified by an organic food certification agency, and has issued an organic food certificate.
  • green peel, long beach fruit, and triploid seedless fruit in Luo Han Guo which is widely planted and contains high content of sweet ingredients such as Luo Han Guo glycosides in the fruit, are selected.
  • the extraction is a continuous countercurrent method or an extraction tank extraction.
  • Luo Han Guo contains about 70% of water, mainly in the pulp, and sweet ingredients such as Luo Han Guo glycosides are mainly concentrated in the pulp, so most of the sweet ingredients in Luo Han Guo can be carried out with the juice by means of juice extraction.
  • the extraction time and the amount of solvent can be significantly reduced, making the extraction more convenient, efficient and efficient.
  • Luo Han Guo fruit seeds contain a large amount of oil and fat components. If the fruit seeds are destroyed during the process of crushing and crushing Luo Han Guo, these oil and fat components will be brought into the extraction solution, which will increase the difficulty for subsequent separation and purification and affect the equipment. And the taste of the product.
  • the squeezed juice method can ensure the integrity of Luo Han Guo seeds.
  • the squeezed fruit juice is directly sent to the subsequent extraction process.
  • the squeezed fruit pulp needs to be dispersed before being sent to the subsequent extraction process to prevent the formation of a solid fruit cake, which affects the extraction efficiency.
  • the squeezed fruit pomace is extracted with water, and the extract is obtained by a continuous countercurrent method.
  • Countercurrent extraction means that during the extraction process, the material and the solvent move continuously at the same time, but the material and solvent move in the opposite direction. The material enters from the end to the end and the solvent enters from the end to the end.
  • the extraction solvent is continuously updated to allow the material Always maintain good mass transfer with solvents.
  • the main characteristics of continuous countercurrent extraction are: short extraction time and low solvent consumption.
  • the countercurrent extraction process for pomace is generally 30-40 minutes. During the extraction process, the ratio of the weight of pomace to the amount of pure water (material-liquid ratio w / w) is 1: 1 to 1: 2.
  • the extraction temperature is between 50 and 90 ° C.
  • the extraction liquid is cooled to below 50 ° C by a plate and frame heat exchanger and sent to the next step. It is further preferred that the temperature during the extraction is about 50 ° C., which does not require a very high temperature, and that the sweet components in the pomace can also be completely extracted.
  • the extraction time of contacting the pomace with pure water is 15-30 minutes, and the ratio of the weight of pomace to the pure water during the extraction process (material-liquid ratio w / w) is 1: 1.
  • the continuous countercurrent extractors are connected in series, and two counter juice extractors are connected in series behind each countercurrent extraction unit, so that the fruit residue can be extracted countercurrently, and then the juice is squeezed.
  • the first juice extraction is the whole fresh Luo Han Guo fruit crushed and squeezed to produce juice and pomace
  • the pulp is mechanically dispersed and then subjected to countercurrent extraction, and finally the juice is extracted to obtain the sweet Luo Han Guo waste residue.
  • the fruit pomace after the second juice extraction in this method allows water containing low-concentration sweetness components to more easily enter the pomace, which can significantly shorten the extraction time.
  • the multi-functional extraction tank can also be used to extract the fruit residue.
  • the extraction is performed 2 to 3 times, each extraction time is 0.5 to 1.5 h, and the extraction temperature is 80 to 100 ° C.
  • the material-liquid ratio w / w is 1: 1 to 1: 2.
  • the extraction solution was filtered by a 200-mesh steel sieve at the bottom of the extraction tank, and cooled by a plate and frame heat exchanger and sent to the subsequent process.
  • the impurity removal specifically includes the following steps: a) centrifugation to remove pulp tissue from the extract solution; b) filtering the centrifugal solution using a ceramic membrane with a pore size of 50-100 nm to obtain a filtrate; c) using macroporous adsorption The resin chromatography column adsorbs impurities in the filtrate.
  • the ceramic membrane is used for filtration.
  • a ceramic membrane with a pore size of 50 to 100 nm is used for filtration, and the temperature of the liquid to be filtered is controlled below 50 ° C.
  • the ceramic membrane with the pore size can significantly retain macromolecular substances and water-insoluble components, while the sweetness of Luo Han Guo Weicheng is able to penetrate the ceramic membrane, thereby removing some impurities.
  • the “adsorption of impurities in the filtrate using a macroporous adsorption resin chromatography column” specifically includes the following steps:
  • step b) Use a polar macroporous adsorption resin chromatography column to adsorb the more polar impurities in the effluent collected in step a): polyphenols, organic acids, etc., and collect the effluent in sections.
  • step b) Wash the chromatographic column in step b) with pure water, and collect the water washing solution in sections, and selectively combine the water washing solution with the effluent collected in the step b). Take the good taste components and concentrate them for purification. Removes ingredients that taste bad.
  • the ceramic membrane permeate is sent to a macroporous adsorption resin chromatography column to further remove impurities and purify the sweet components of Luo Han Guo.
  • macroporous resins are able to adsorb mogrosides, but the adsorption capacity is different.
  • Non-polar and weakly polar macroporous resins have relatively large amounts of mogrosides. Porous resin adsorption is relatively small. Compared with the sweet components in Luo Han Guo, non-polar or weakly polar macroporous resins are more likely to adsorb less polar flavonoids, water-soluble fatty acids, and no sweet or even bitter terpenoids. : Triterpenoid aglycones of Mogroside, Mogroside I, Mogroside II, Mogroside III.
  • the non-polar macroporous adsorption resin is preferably D101 and / or LX-60.
  • the weakly polar macroporous adsorption resin is preferably HPD-722 and / or AB-8.
  • the polar macroporous resin is preferably LX-17, and more preferably LX-17 with a mesh number of 60-120.
  • the volume-to-mass ratio (L / kg) of the amount of resin in the non-polar macroporous adsorption resin column to the total amount of Luo Han Guo is preferably 1: 2 to 1: 5, and the flow rate is preferably 1 to 3 BV / h.
  • the volume mass ratio (L / kg) of the amount of the resin in the polar macroporous adsorption resin column to the mogroside V in the upper column liquid is preferably 50: 1 to 200: 1.
  • Non-polar or weakly polar macroporous adsorption resin chromatography columns continue to be used under the condition that a large amount of mogroside V has been adsorbed, mogroside V has begun to leak in the effluent, and the amount of mogroside V adsorbed by the resin column tends to be saturated.
  • the ceramic membrane filter is put on the column, and the resin chromatography column can still adsorb the sweet components of non- Luo Han Guo. After the mogroside V reaches saturation in the resin, as the filtrate continues to be applied to the column, more impurities are adsorbed, and the mogroside V adsorbed in the resin will be replaced by other impurities.
  • the type of the polar macroporous resin is LX-17, and more preferably, the polar macroporous resin chromatography column equipped with the model LX-17 with a mesh number of 60-120 is used to adsorb impurities.
  • the highly polar impurity components will be adsorbed by the polar macroporous adsorption resin. It is difficult for water to decompose these components.
  • the sweeteners of Luo Han Guo are not easily adsorbed, and they are easy to be carried on. Directly flowing out from the aqueous solution, the mogrosides in the sweet taste component of Luo Han Guo will be adsorbed by the polar macroporous resin and desorbed by the aqueous solution.
  • the polar macroporous adsorption resin can perform chromatographic purification of mogrosides.
  • components with high content such as mogroside V collected in the sections, the bad taste collected in the sections can be removed.
  • Mogroside III and mogroside IIe are high in components, which further reduce the content of ingredients that affect taste.
  • the “concentration purification” in the present invention specifically includes the following steps: using a nanofiltration membrane with a pore size of 1 to 2 nm to purify and remove impurities from the solution.
  • Nanofiltration membrane materials are generally cellulose acetate, sulfonated polysulfone, sulfonated polyethersulfone, polyvinyl alcohol, polyamide, ceramics, metals, and the like.
  • a ceramic film having a pore diameter of 1-2 nm is used. Removes most of water, inorganic salts, amino acids, monosaccharides, disaccharides, organic acids, etc.
  • the nanofiltration membrane retentate will still contain inorganic salts, amino acids, monosaccharides, disaccharides, organic acids and other components.
  • the concentrated solution needs to be diluted again with an appropriate amount of pure water, and the nanofiltration is concentrated and purified again. Repeat several times to remove the inorganic salt, amino acid, monosaccharide, disaccharide, organic acid and other components. Further preferably, 2 times the volume of pure water of the concentrated solution is put in each time, and the process is repeated 1-4 times.
  • the solid content w / w of the concentrated liquid obtained by the nanofiltration membrane retention is only about 10% to 20%. If the moisture content is too high, it is easy to breed microorganisms and not easy to store. Therefore, other concentration methods need to be used to make the concentrated solution thicker and more convenient for storage and transportation.
  • a multifunctional vacuum concentration tank is used, with a temperature of about 65 ° C and a vacuum of about -0.08 MPa. Concentrate to 60Brix to 70Brix extract.
  • the concentrated liquid needs to be further dried to obtain a powder or a solid.
  • a centrifugal spray drying tower is used for drying, the solid content of the feed is about 30%, the rotation speed of the atomizer is 20,000 r / min, the inlet air temperature is 180 ° C, and the outlet air temperature is 95 ° C, so that the bulk density (bulk density) is obtained. 20g / 100ml to 50g / 100ml of Luo Han Guo sweet taste composition powder.
  • a vacuum drying box is used for drying, and the solid content of the feed is about 50%, the temperature is about 65 ° C., and the degree of vacuum is about -0.09 MPa.
  • the obtained Luo Han Guo sweet taste composition exists as an internal fluffy irregular solid. You can also use a freeze vacuum dryer, a boiling dryer, a circulating hot air dryer, and so on.
  • the method of the present invention is suitable for large-scale production of Luo Han Guo sweet taste composition, and is also suitable for producing organic Luo Han Guo sweet taste composition from organic Luo Han Guo raw material. Different batches and different raw materials produced by the same raw material (different between ordinary Luo Han Guo and organic Luo Han Guo) The specifications of Luo Han Guo sweet taste composition can be mixed to meet the market requirements for specific content (such as 25% Luo Han Guo V, 80% Luo Han Guo V, etc.).
  • a second object of the present invention is to provide a compound sweetener (composite sweetener).
  • the compound sweetener may be the following composition A or a mixture of the composition A and the composition B.
  • Composition A Luo Han Guo raw material Luo Han Guo sweetness composition obtained by the method described in "A method for preparing Luo Han Guo sweetness composition from Luo Han Guo" above, the main component of the sweet taste composition comprises 10% to 85% Mogroside V, 0.2% to 2% Mogroside VI, 1% to 12% 11-O-Mogroside V, 0.5% to 5% isomogroside V, 0.1% to 3% siamidine I, 0.1% to 3 % Mogroside IVa, 0.2% to 3% Mogroside IVe, 0% to 12% sucrose, 0% to 8% fructose, 0% to 6% glucose, 0% to 10% mannitol, and mogroside III ⁇ 0.5% , Mogroside IIe ⁇ 0.1%,
  • Composition B one or more ingredients, which may be sweeteners, flavors, flavors, flavors, pigments, plant extracts, excipients, and the like.
  • the compound sweetener is Composition A
  • the raw materials used are green peel, long beach fruit and triploid seedless Luo Han fruit in ordinary Luo Han Guo.
  • the compound sweetener is Composition A
  • the raw materials used are organic green peel fruit, organic long beach fruit, and organic triploid seedless Luo Han fruit in organic Luo Han Guo.
  • the compound sweetener is component A, and contains 75% to 83% mogroside V, 0.4% to 1% mogroside VI, 8% to 12% 11-O-mogroside V, 2.5% to 4% iso-mogroside V, 1.5 to 2% siamoside I, 0.5% to 2% mogroside IVa, 1% to 2% mogroside IVe, mogroside III 0%, and mogroside IIe 0%, sucrose, fructose, glucose, mannitol are all 0%.
  • the compound sweetener contains off-flavored and bitter-grossing Luo Han Guo glycoside III and Luo Han Guo glycoside II content is basically 0, and does not contain energetic sugars such as monosaccharides and disaccharides, and has high sweetness and sweetness. Pure, no odor, ultra-low calories.
  • the compound sweetener is component A, and contains 47% to 54% mogroside V, 1% to 1.6% mogroside VI, and 5% to 8% 11-O-mogroside.
  • V 2.5% to 4% iso-mogroside V, 1.5 to 2% siamoside I, 0.5% to 2% mogroside IVa, 1% to 2% mogroside IVe, mogroside III ⁇ 0.2%
  • mogroside IIe is 0%, 0.1% to 1% sucrose, 0.1% to 1% fructose, 0.1% to 1% glucose, 0.1% to 1% mannitol.
  • the compound sweetener still contains a small amount of total mango glycoside III and total mango glycoside II, so retaining a small amount of sugars such as sucrose, fructose, glucose, and mannitol can enhance the pre-sweetness of the compound sweetener and can Reduces off-flavors and makes the taste closer to sucrose.
  • the compound sweetener is component A, and contains 23% to 28% mogroside V, 0.2% to 0.6% mogroside VI, 2% to 4% 11-O-mogroside V, 1% to 2% iso-mogroside V, 0.3 to 1% siamoside I, 0.5% to 1% mogroside IVa, 0.5% to 1% mogroside IVe, mogroside III ⁇ 0.5%, mogroside IIe ⁇ 0.1%, 2% to 6% sucrose, 2% to 4% fructose, 1% to 4% glucose, 1% to 4% mannitol.
  • the compound sweetener still contains a small amount of Luo Han Guo glycoside III and Luo Han Guo glycoside II, so retaining the appropriate amount of sucrose, fructose, glucose, mannitol and other raw materials such as Luo Han Guo can make the compound sweet.
  • the front sweetness of the agent is stronger, which can play a role in appropriately reducing bitterness, masking off odors, and making the taste closer to sucrose.
  • the sweetening preparation may exist in a powder form, and the bulk density (bulk density) of the powder is 20 g / 100ml to 50g / 100ml. Within such a bulk density range, the sweetening preparation powder can Quickly dissolve in water, 1g can be completely dissolved in 100ml of water at normal temperature in 30-50 seconds.
  • the powder has a low to high content of mogroside V in the sweetness composition, and the color ranges from yellow to light yellow, to off-white, and finally to pure white.
  • the sweet-grossing composition of Luo Han Guo may also exist in a liquid form.
  • the liquid varies from low to high content of mogroside V in the sweet composition, and the color ranges from brown to yellow, to light yellow, and finally to colorless.
  • the Luo Han Guo sweet taste composition is in the form of an aqueous solution of 60-70 Brix.
  • the sweetness composition may also be present in an irregular solid form, preferably in the form of an internal fluffy solid.
  • the third object of the present invention is to provide foods, beverages, health products, daily chemicals, medicines, and the like containing the sweetness composition described above.
  • the invention effectively controls the content of mogroside III and IIe through a specific preparation method, so that the sweet taste composition of mogroside is better, and only pure water and no ethanol are used in the preparation process of the sweet taste composition of the present invention.
  • Such as organic solvents the production process is more green and healthy.
  • Example 2 is an HPLC chart of the sweet taste composition obtained in Example 1;
  • Example 3 is an HPLC chart of the sweet taste composition obtained in Example 2;
  • Example 4 is a HPLC chart of the sweet taste composition obtained in Example 3.
  • FIG. 5 is a powder HPLC chart of the sweet taste composition obtained in Example 2 and Comparative Example 1.
  • FIG. 5 is a powder HPLC chart of the sweet taste composition obtained in Example 2 and Comparative Example 1.
  • This embodiment provides a method for preparing a sweet-scented composition of Luo Han Guo from Luo Han Guo, which specifically includes the following steps:
  • Ripening Choose ripe golden yellow Luo Han Guo with a weight of 300 kg and 1200 kg Qing Luo Han Guo (fruit age is more than 3 months) and arrange them in a crosswise arrangement of weight 1: 4 to ensure that the ethylene released by mature Luo Han Guo can fully contact with Qing Luo Han Guo.
  • the covered plastic film separates Luo Han Guo from the outside air, which maintains the high concentration of ethylene and maintains heat. After ripening at a temperature of 25 to 38 ° C for 3 days, the covered plastic film is removed, and the ventilation is good at room temperature.
  • Nanofiltration The combined 900L of liquid was subjected to nanofiltration using a ceramic membrane with a pore size of 1 nm. Concentrate until the retentate is about 100L, add 200L of pure water to dilute, and continue nanofiltration to concentrate to about 100L. The process of dilution and concentration is repeated 3 times to obtain 100L of colorless transparent liquid.
  • Step 6 The remaining paragraphs 3-6 and 10-12 are combined in a total of 2100L in the process of adsorbing impurities, and then sent to the nanofiltration process and then concentrated and dried to obtain about 35% of mogroside V product, or each stage can be separately subjected to sodium absorption. Filtration, concentration, and drying yield 10% to 65% products of mogroside V of different specifications. It is also possible to combine these sections and add the next batch to reload the polar resin column to obtain a higher content of product.
  • This embodiment provides a method for preparing a sweet-scented composition of Luo Han Guo from Luo Han Guo, which specifically includes the following steps:
  • Nanofiltration The above-mentioned combined 2400L liquid was subjected to nanofiltration using a ceramic membrane with a pore size of 2nm. Concentrate to about 100L of retentate, add 200L of pure water to dilute, and continue nanofiltration to concentrate to about 100L. After this process of dilution and concentration is repeated 2 more times, 100L of slightly yellow transparent liquid is obtained.
  • This embodiment provides a method for preparing a sweet-scented composition of Luo Han Guo from Luo Han Guo, which specifically includes the following steps:
  • Extraction 1050kg of scattered fruit residue is extracted with a multi-functional extraction tank. Extraction is performed 3 times, the first extraction is 1.5h, the extraction temperature is 100 ° C, the second and third extraction times are 1h, and the temperature is 80 ° C. The amount of pure water used for each extraction is 2100L. The extraction solution was filtered through a 200-mesh steel sieve at the bottom of the extraction tank. The combined extraction solutions were combined for a total of 5700 L and cooled to about 50 ° C through a plate and frame heat exchanger and sent to the centrifugation process.
  • Nanofiltration The above-mentioned combined 4800L liquid was subjected to nanofiltration using a ceramic membrane with a pore size of 2 nm. Concentrate until the retentate is about 200L, add 400L of pure water to dilute, and then continue nanofiltration to concentrate to about 200L. After this process of dilution and concentration is repeated once more, 200L of yellow transparent liquid is obtained.
  • the Luo Han Guo triterpenoid glycosides were prepared from the fresh fruits of Luo Han Guo to obtain a slightly yellow powder.
  • the powders obtained in Examples 1, 2, 3 and Comparative Example 1 were added to pure water to prepare a solution having the same concentration of mogroside V (mogroside V concentration of 0.5 mg / ml).
  • 20 people (10 men and 10 women, age The post-bitter tasting group composed of paragraphs 20-61) blindly tested the above 4 different solutions and then scored.
  • the tasting method was to rinse the mouth with pure water first, and then fully contact the solution to be tasted with the tongue and mouth for 10s. Then swallow (for easy access to the solution deep in the base of the tongue), then score, gargle before the next tasting, and at least 1 minute between the two tastings.
  • the scoring criterion is that the lower the bitter taste, the higher the score, and the stronger the later bitter taste.
  • the sweet taste composition of Luo Han Guo obtained in 1, 2 and 3 contains sugars such as sucrose, fructose, glucose, and mannitol, but not in Example 1.
  • sugars such as sucrose, fructose, glucose, and mannitol
  • the content of mogroside V in the comparative example is similar to that in Example 2, but does not contain these saccharides.
  • About 10-60% of Mogroside V products with a small amount of monosaccharides and disaccharides can have a rich sweetness and make the taste closer to sucrose; 2.
  • Mogroside IIe is not included in all the examples, and mogroside The higher the content of V, the smaller the content of mogroside III.
  • the content of mogroside III is 0%, and the peaks of mogroside IIIe and mogroside IIIa1 are not seen in the spectrum. These substances have a bad taste or even have a strong bitter taste. The less the score, the higher the score of the mouthfeel evaluation; 3.
  • the content of Mogroside V in Example 2 and Comparative Example 1 are similar, and the polarity in Example 2 is slightly weaker than that of Mogroside V.
  • the compounds are siamidine I and mogroside IVa, The content of mogroside IVe is lower than that of comparative example 1, and does not contain mogroside III and mogroside IIe, which are less polar than mogroside IV.
  • Mogroside V adsorbs saturated non-polar or weakly polar resins, which can significantly absorb mogroside III and mogroside II, reduce or even remove components with bad taste, and improve the taste of the product, but this method can also Mangosteen total glycosides IV attachment portion (siamenoside I, mogroside IVa, mogroside IVe, etc.) may improve the bitter glycoside and total glycosides IV Luohanguo separated by a subsequent process, so that the development of new products.
  • the invention provides a method for preparing a sweet-scented Luo Han Guo composition from the Luo Han Guo and application thereof.
  • the method for extracting the sweetness composition from Luo Han Guo provided by the present invention preferably includes the following steps: ripening the immature Luo Han Guo, extracting the juice through pure water, removing impurities, concentrating and purifying to obtain a sweet taste composition.
  • the present invention also provides a compound sweetener containing the above-mentioned sweetness composition.
  • the compound sweetener can be widely used in food, beverages, health products, and daily chemicals.
  • the sweet taste composition of mogroside is better, and only pure water and organic solvents such as ethanol are not used in the preparation process of the sweet composition of the present invention.
  • the production process is more green and healthy, and has better economic value and application prospects.

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Abstract

一种从罗汉果中制备罗汉果甜味组合物的方法及其应用。该从罗汉果中提取甜味组合物的方法优选包括如下步骤：对未成熟的罗汉果进行催熟，通过榨汁、纯水提取，去除杂质，浓缩纯化等步骤得甜味组合物。还包括含有上述甜味组合物的复配甜味剂，可广泛应用于食品、饮品、保健品、日化用品中。通过控制罗汉果苷III、罗汉果苷IIe等含量，使得罗汉果甜味组合物的味道更好，且甜味组合物的制备过程中只用到纯水、不使用乙醇等有机溶剂，生产过程更加绿色健康。

Description

一种从罗汉果中制备罗汉果甜味组合物的方法及其应用
交叉引用
本申请要求2018年9月6日提交的专利名称为“一种从罗汉果中制备罗汉果甜味组合物的方法及其应用”的第201811039595.6号中国专利申请的优先权，其全部公开内容通过引用整体并入本文。
技术领域
本发明属于植物有效成分提取分离技术领域，更具体地，涉及一种从罗汉果中制备罗汉果甜味组合物的方法，还涉及一种含有由上述方法获得的罗汉果甜味组合物的复配甜味制剂。
背景技术
罗汉果Siraitia grosvenorii(Swingle)C.Jeffrey(曾被称为Momordica grosvenorii)，又名光果木鳖，是葫芦科多年生藤本植物的果实。雌雄异株，夏季开花，秋季结果。主要产于中国广西桂林，湖南永州、邵阳、怀化，广东等地，罗汉果有青皮果、长滩果、冬瓜果、拉江果、红毛果、油桐果等品种，青皮果种植较多，近几年也有种植地种植无籽罗汉果(三倍体无籽罗汉果、单性结实无籽罗汉果)。罗汉果也是国家首批批准的药食两用材料之一，其主要功效是能润肺止咳、生津化痰。罗汉果中的主要甜味成分是是一类以罗汉果醇这种葫芦素烷三萜为苷元的皂苷，这些皂苷为有甜味皂苷(含有4个或者4个以上葡萄糖基团)和没有味道或者有杂味及苦味的皂苷(含有3个及3个以下葡萄糖基团)。有甜味的罗汉果皂苷有11-O-罗汉果苷V，新罗汉果苷，罗汉果苷V，异罗汉果苷V，赛门苷I，罗汉果苷VI、罗汉果苷IVe、罗汉果苷IVa等；没有味道或者味道苦涩的有罗汉果总苷III(包括罗汉果苷III、罗汉果苷IIIa1、罗汉果苷IIIe、罗汉果苷IIIe等)、罗汉果总苷II(包括罗汉果苷IIe、罗汉果苷IIa、罗汉果苷IIa1、罗汉果苷IIe、罗汉果苷IIb、11-O-罗汉果苷IIe等)、罗汉果苷总I(包括罗汉果苷Ia1、罗汉果苷Ie1等)，在这些皂苷中，罗汉果 苷V的含量最高，罗汉果苷V具有稳定性好、卡路里几乎为零、甜度高达蔗糖的250-300倍、甜味持续时间长、无后苦味、无后涩味等特点，作为一种天然的甜味剂，已经广泛地应用在了高档饮料、食品、保健品中，且被越来越多的人所认可，在降糖的国际背景中地位越来越明显。
公开号为CN101007042B中介绍了一种脱色、脱苦的罗汉果提取物的制备方法，采用14倍水侵泡煎煮罗汉果，然后树脂吸附乙醇解吸得产品。公开号为CN103923152B的一种罗汉果甙V的提取方法中，以罗汉果鲜果为原料，经清洗、破碎，糖化鲜罗汉果，提取，然后沉降离心处理，大孔树脂吸附、分离，采用多树脂柱组选择吸附，并分部收集解吸液，根据含量不同，分批次合并处理，离子交换树脂精制，浓缩、回收乙醇，硅胶精制，浓缩和喷雾干燥得成品。美国专利US6124442提供一种用罗汉果制备含有罗汉果甜苷的干燥组合物，提取所得液体与具有氧化值得溶液混合，然后沉淀，澄清液果大孔树脂，然后用醇洗脱树脂，获得的解吸液浓缩干燥得含有三萜苷的干燥组合物。美国专利US 20110021456提供一种来源于罗汉果的无苦味杂质，浅色的甜味组合物制备方法，先提取，再澄清，然后用大孔树脂吸附罗汉果甜苷，使用梯度的乙醇解吸，加热生成类黑精，再用离子交换树脂脱色。美国专利US2014044843A1中提供的罗汉果甜汁制备方法，先提取，再澄清，然后用阴离子交换树脂与阳离子交换树脂对提取液进行纯化，得到味道纯正的甜汁组合物。
以上制备罗汉果甜苷的发明大多采用长时间储存让罗汉果成熟，或者用到酶制剂加入罗汉果提取液中加快罗汉果糖化过程，然后用大孔吸附树脂对罗汉果甜苷进行吸附，然后用醇溶液对罗汉果甜苷进行解吸，从而起到浓缩或者纯化的作用，再通过离子交换树脂去除多酚黄酮等有色杂质同时调节至适宜的酸碱度。这样工艺中会用到外源酶，纯化过程中会用到乙醇等溶剂，而且使用离子交换树脂去除有色物质的过程是一个化学反应过程，会对除了罗汉果甜苷外的其他留在产品中的成分产生影响，这些工序都会对有机罗汉果提取物的生产制造障碍。而且这样的工艺过程中所得的 产品中的罗汉果苷III、罗汉果苷IIe罗汉果苷Ia1以及这些成分的同分异构体含量仍然很高，这些成分含有不好的味道。
发明内容
本发明的第一目的在于提供一种从罗汉果中提取甜味组合物的方法，该方法包括如下步骤：
将成熟的罗汉果与未成熟的罗汉果按重量比为1:4～1:8放置在一起，在25～38℃下密封2～4天，再将其置于通风环境下1～4天得到罗汉果原料，将所述罗汉果原料榨汁得汁夜和果渣，合并所述汁液和使用纯水提取所述果渣后的提取液，除杂，浓缩纯化，即得。
种植园采摘罗汉果时基本上以的果柄发黄与否，来判断罗汉果是否可以采摘，按照经验，果柄发黄说明罗汉果的果龄(从果实形成至采摘果实的生长时间)超过3个月，达到了可以采摘的要求，但是这些采摘了的罗汉果大部分依然是青色或者果皮表面只有部分呈现出淡黄色，这样的鲜果中主要的甜味成分如罗汉果苷V，罗汉果苷VI，11-O-罗汉果苷V，异罗汉果苷V等仍然没达到最高的含量，而且果实中仍然含有部分有苦味的罗汉果苷IIe，11-O-罗汉果苷II，罗汉果苷Ia1等，而且酸涩味的成分含量也会很高，一般需要2周左右才能通过罗汉果自身的生物转化，提高有甜味的罗汉果甜苷的含量。
优选地，本发明通过成熟罗汉果自身产生的乙烯对青罗汉果进行催熟，催熟方法包括：a)通过挑选熟透了的外表为金黄色罗汉果与青罗汉果按照适当的重量交叉排列放置，保证成熟罗汉果释放的乙烯能与青罗汉果充分接触，成熟罗汉果与青罗汉果的重量比为1:4～1:8。在能起到维持乙烯高浓度与保温的作用的密闭环境下，温度在25至38℃范围内催熟2至4天。b)然后将其放置于通风良好的环境中，室温下放置1～4天，在空气的条件下能保证果皮表面干燥防止长霉且罗汉果能充分有氧呼吸，有利于罗汉果中生物转化过程。
优选地，通过直接通入乙烯气体的方法进行催熟，密闭条件下，温度 在25至38℃范围内，乙烯浓度为500ppm到1500ppm范围内，催熟2至4天后，将其置于通风环境中，室温下再次放置1～4天。
通过上述3-8天催熟，罗汉果鲜果的生青味，酸涩味，苦味现象得到明显的改善，甜味明显增强。罗汉果鲜果中有苦味的罗汉果苷类成分与无甜味的罗汉果苷类成分的含量明显降低，其中罗汉果苷III，罗汉果苷IIe的含量能降低到原来水平的10％以下。能将原料中的罗汉果苷V和11-O-罗汉果苷V的含量提升到原来含量的180％左右。
本发明使用的罗汉果鲜果可为葫芦科藏瓜族中罗汉果属中的罗汉果亚属和无鳞罗汉果亚属，也可为多倍体罗汉果和无籽罗汉果。罗汉果亚属有罗汉果Siraitia grosvenorii(Swingle)C.Jeffrey ex Lu et Z.Y.Zhang，主要产广西、贵州、湖南南部、广东和江西；翅子罗汉果Siraitia siamensis(Craib)C.Jeffrey ex Zhong et D.Fang，产广西西部和云南东南部，在越南北部和泰国也能找到。无鳞罗汉果亚属有无鳞罗汉果Siraitia borneensis(Merr.)C.Jeffrey ex Lu et Z.Y.Zhang，产于广东、云南(西畴)及西藏(墨脱)，泰国、马来西亚也有；无鳞罗汉果(原变种)Siraitia borneensis(Merr.)C.Jeffrey ex Lu et Z.Y.Zhang var.Borneensis；裂叶罗汉果Siraitia borneensis(Merr.)C.Jeffrey ex Lu et Z.Y.Zhang var.lobophylla A.M.Lu et Z.Y.Zhang产于云南绿春；云南罗汉果Siraitia borneensis(Merr.)C.Jeffrey ex Lu et Z.Y.Zhang var.yunnanensis A.M.Lu et Z.Y.Zhang产云南峨山；台湾罗汉果Siraitia taiwaniana(Hayata)C.Jeffrey ex Lu et Z.Y.Zhang产于台湾。
有机罗汉果是指在罗汉果的种植生长过程中严格按照有机生产规程，禁止使用任何化学合成的农药、化肥、生长调节剂等化学物质，禁止使用基因工程及其产物，而是遵循罗汉果生长的自然规律和生态学原理，且经过有机食品认证机构鉴定认证，并颁发有机食品证书的罗汉果。
优选地，本发明选用被广泛种植，而且果实中罗汉果甜苷等甜味成分含量高的罗汉果中的青皮果、长滩果与三倍体无籽果，更加优选地，选用有机青皮果、有机长滩果与有机三倍体无籽罗汉果。
在本发明中，所述提取为连续逆流法或提取罐提取。
罗汉果中含有70％左右的水分，主要在果肉中，而罗汉果甜苷等甜味成分也主要集中在果肉中，因此可以通过榨汁的方式，将罗汉果中大部分甜味成分随果汁携带出来。剩下的果渣提取时，能显著减少提取时间与溶剂用量，让提取更加方便快捷高效。罗汉果果籽中含有大量的油脂成分，如果在罗汉果被破碎和压榨的过程中果籽被破坏，这些油脂成分便会带入到提取液中，为后续的分离纯化增加难度，也会影响到设备及产品的口感。采用挤压榨汁方式，可以保证罗汉果果籽的完整性。压榨出的果汁直接送往提取后面的工序，挤压榨汁后的果渣在送往后续提取工序前需要进行分散，防止形成结实的果渣饼，影响提取的效率。
压榨后的果渣用水进行提取，使用连续逆流法进行提取得提取液。逆流提取是指在提取的过程中，物料和溶剂同时连续运动，但物料与溶剂的运动方向相反，物料从首端进从末端出，溶剂从末端进首端出，提取溶剂不断更新，让物料与溶剂一直保持良好的传质过程。连续逆流提取的主要特点是：提取时间短，溶剂用量少。对果渣的逆流提取过程一般为30～40min，提取过程中果渣重量与纯水的用量比(料液比w/w)为1:1～1:2。提取温度在50～90℃之间。提取液用板框热交换器冷却至50℃以下，送往下一工序。进一步优选地是，提取过程中温度为50℃左右，不需要很高的温度，果渣中的甜味成分也能提取完全。果渣与纯水接触的提取时间为15～30min，提取过程中果渣重量与纯水的用量比(料液比w/w)为1:1。
在本发明一个优选实施方式中，在上述连续逆流法中采用两台连续逆流提取机串联，每台逆流提取机组后面再串联两台挤压榨汁机，让果渣得以逆流提取，然后榨汁，第二次榨汁(第一次榨汁为完整的罗汉果鲜果破碎挤压榨汁，生产果汁与果渣)的果渣机械分散再经过逆流提取，最后榨汁得到没有甜味的罗汉果废渣。该方法中第二次榨汁后的果渣能让含低浓度甜味成分的水更容易进入到果渣中，能显著缩短提取时间。
在本发明一个优选实施方式中，也可以使用多功能提取罐对果渣进行 提取，提取2～3次，每次提取时间为0.5～1.5h，提取温度为80-100℃，每次提取的料液比w/w为1:1～1:2。提取液在提取罐底部得到200目钢筛过滤，并经过板框热交换器冷却送往后续工序。
在本发明中，所述除杂具体包括如下步骤：a)离心去除所述提取液中果肉组织；b)将离心液使用孔径为50～100nm的陶瓷膜过滤得滤液；c)使用大孔吸附树脂层析柱吸附所述滤液中的杂质。
罗汉果挤压榨汁所得的果汁及提取液中残留大量的果肉组织，直接去用陶瓷膜过滤得话，会加大陶瓷膜的负担，显著提高陶瓷膜清洗的频率，因此要去除这些果肉组织。通常使用离心方法，可以使用卧螺离心机、碟式离心机、管式离心机。优选地，使用卧螺离心机，转速2000～3000r/min进行离心，卧螺离心机转速合适，处理量大，清洗方便，能显著清除果肉组织。
为去除挤压榨汁所得的果汁中及提取液中的悬浮颗粒，原果胶，植物纤维，大分子蛋白质，大分子多糖，果胶等物质，使用陶瓷膜进行过滤。优选地，使用孔径为50～100nm的陶瓷膜进行过滤，待过滤的液体温度控制在50℃以下，该孔径的陶瓷膜能显著地截留大分子物质及不溶于水的成分，而罗汉果中的甜味成能够透过陶瓷膜，从而实现去除部分杂质的作用。
本发明中，所述“使用大孔吸附树脂层析柱吸附所述滤液中的杂质”具体包括如下步骤：
a)使用非极性大孔吸附树脂层析柱或者弱极性大孔吸附树脂层析柱吸附滤液中极性比罗汉果主要甜味成分弱的物质：罗汉果苷III、罗汉果苷IIe、罗汉果苷Ia1等味道不好的杂质，从有罗汉果苷V有泄露时开始收集流出液。
b)使用极性大孔吸附树脂层析柱吸附步骤a)中收集的流出液中的极性较强的杂质：多酚、有机酸等，分部收集流出液。
c)用纯水洗步骤b)中的层析柱，分部收集水洗液，选择性地合并 水洗液与步骤b)中分部收集的流出液，取口感好的组分送去浓缩纯化，舍去口感不好的组分。
陶瓷膜透过液送往大孔吸附树脂层析柱进一步去除杂质纯化罗汉果甜味成分。一般情况下，大孔吸附树脂都能够吸附罗汉果甜苷，只是吸附容量有差别，非极性与弱极性大孔吸附树脂对罗汉果甜苷的吸附量相对较大，中极性与极性大孔吸附树脂吸附量相对较小。相对于罗汉果中的甜味成分，非极性或者弱极性的大孔吸附树脂更容易吸附极性更小的黄酮类物质，水中微溶的脂肪酸，没有甜味的甚至有苦味的萜类物质：如罗汉果甜苷的三萜苷元、罗汉果总苷I、罗汉果总苷II、罗汉果总苷III。
其中，所述非极性大孔吸附树脂优选型号为D101和/或LX-60。所述弱极性大孔吸附树脂优选型号为HPD-722和/或AB-8。所述极性大孔树脂优选型号为LX-17，更加优选地为60-120目数的LX-17。
所述非极性大孔吸附树脂柱中的树脂用量与所述罗汉果总量的体积质量比(L/kg)优选为1:2～1:5，流速优选为1～3BV/h。
所述极性大孔吸附树脂柱中的树脂用量与上柱液中罗汉果苷V的体积质量比(L/kg)优选为50:1～200:1。
非极性或者弱极性大孔吸附树脂层析柱在已经吸附大量罗汉果苷V、流出液中已经开始有罗汉果苷V泄露、树脂柱对罗汉果苷V的吸附量趋向于饱和的情况下继续用陶瓷膜过滤液上柱，树脂层析柱仍然能吸附非罗汉果甜味成分。罗汉果苷V在树脂中达到饱和后，随着过滤液继续上柱，更多的杂质被吸附，树脂中吸附的罗汉果苷V会被其他杂质成分替换下来。取同样体积的流出液与上柱液，加入相同重量的辅料浓缩干燥后，发现流出液中罗汉果苷V及11-O-罗汉果苷V的含量有明显的升高，而罗汉果苷III及罗汉果苷IIe的含量显著减少。且流出液的口感明显比上柱液少了舌根所能感受到苦味及后苦味。从罗汉果苷V有泄露开始收集流出液，至相应的滤液完全经过层析柱。
在本发明中，使用极性大孔吸附树脂柱吸附上文所述的流出液中的极 性较强的杂质，所用树脂体积(L)与上柱液中罗汉果苷V的重量(kg)比＝50:1～200:1，速为1～3BV/h，然后用纯水洗极性大孔吸附树脂层析柱，分部收集流出液与水洗液。优选地所述极性大孔树脂优选型号为LX-17，进一步优选地，为使用装有目数为60-120的型号LX-17的极性大孔吸附树脂层析柱吸附杂质。
这些非极性或者弱极性树脂中收集的流出液中杂质大多为多酚类物质，部分有机酸类物质，部分极性较强的黄酮苷，部分小分子蛋白质，部分肽类及部分氨基酸等。极性强的杂质成分会被极性大孔吸附树脂吸附，水很难将这些成分解吸出来，罗汉果甜味成分中的单糖、双糖、部分氨基酸等不被容易被吸附，很容易携带在水溶液中直接流出，罗汉果甜味成分中的罗汉果甜苷则既会被极性大孔树脂吸附，又会被水溶液解吸出来，因而在极性大孔树脂与水溶液间动态的被吸附与被解吸，从而极性大孔吸附树脂能对罗汉果甜苷起到层析纯化的作用，通过选择性地合并分部收集到的罗汉果苷V等含量高的组分，去掉分部收集到的味道不好的罗汉果苷III及罗汉果苷IIe含量高的组分，进一步降低产品中影响口感的成分的含量。
本发明所述的“浓缩纯化”具体包括如下步骤：使用孔径为1～2nm的纳滤膜纯化去除杂质后的溶液。纳滤膜材料一般为醋酸纤维素、磺化聚砜、磺化聚醚砜、聚乙烯醇、聚酰胺、陶瓷、金属等。优选地，使用孔径为1-2nm的陶瓷膜。去除大部分水分，无机盐，氨基酸，单糖，双糖，有机酸等。
在纳滤浓缩后，纳滤膜截留液中仍然会含有无机盐，氨基酸，单糖，双糖，有机酸等成分，通常会需要重新用适量的纯水稀释浓缩液，再次纳滤浓缩纯化，重复多次才能将无机盐，氨基酸，单糖，双糖，有机酸等成分除去。进一步优选地，每次放入2倍浓缩液体积的纯水，重复1-4次。
通常，纳滤膜截留所得浓缩液固形物含量w/w只有10％至20％左右，水分含量太高容易滋生微生物，不容易储存。因此需要用其他浓缩方法将 浓缩液变得更加浓稠方便储存与运输，在本发明一个优选实施方式中，使用多功能真空浓缩罐，温度65℃左右，真空度-0.08MPa左右，将截留液浓缩成60Brix至70Brix浸膏。
为满足市场的需要，需要进一步将浓缩液进行干燥，以获得粉末或者固体。优选地，使用离心式喷雾干燥塔进行干燥，进料固形物含量为30％左右，雾化器转速为20000r/min，进风温度180℃，出风温度95℃，得到堆积密度(松密度)为20g/100ml至50g/100ml的罗汉果甜味组合物粉末。备选地，使用真空干燥箱进行干燥，进料固形物含量50％左右，温度65℃左右，真空度-0.09MPa左右，得到的罗汉果甜味组合物以内部蓬松的无规则固体形式存在。也可以用冷冻真空干燥机，沸腾干燥机，循环热风干燥机等干燥。
本发明方法适合大规模生产罗汉果甜味组合物，同样也适合于用有机罗汉果原料生产有机罗汉果甜味组合物，同样(普通罗汉果和有机罗汉果区别开来)的原料生产出来的不同批次及不同规格的罗汉果甜味组合物可以进行混合，从而满足市场对特定含量(比如25％罗汉果苷V，80％罗汉果苷V等)的要求。
本发明的第二目的在于提供一种复配甜味剂(复合甜味剂)，这种复配甜味剂可以是下列的组合物A，也可以是组合物A与组合物B的混合物。
组合物A：罗汉果原料通过上文“一种从罗汉果中制备罗汉果甜味组合物的方法”所描述的方法获得的罗汉果甜味组合物，该甜味组合物的主要成分包括10％到85％罗汉果苷V，0.2％到2％罗汉果苷VI，1％到12％11-O-罗汉果苷V，0.5％到5％异罗汉果苷V，0.1％到3％赛门苷I，0.1％到3％罗汉果苷IVa，0.2％到3％罗汉果苷IVe，0％到12％蔗糖，0％到8％果糖，0％到6％葡萄糖，0％到10％甘露醇，且罗汉果苷III≤0.5％，罗汉果苷IIe≤0.1％，
组合物B：一种或多种成分，这些成分可以是甜味剂、香精香料、调 味剂、色素、植物提取物、赋形剂等。
优选地，复配甜味剂是组合物A，所用原料为普通罗汉果中的青皮果、长滩果及三倍体无籽罗汉果。
更加优选地，复配甜味剂是组合物A，所用原料为有机罗汉果中的有机青皮果、有机长滩果及有机三倍体无籽罗汉果。
在一些优选的实施方式中，复配甜味剂是组分A，且其中含有75％到83％罗汉果苷V，0.4％到1％罗汉果苷VI，8％到12％11-O-罗汉果苷V，2.5％到4％异罗汉果苷V，1.5到2％赛门苷I，0.5％到2％罗汉果苷IVa，1％到2％罗汉果苷IVe，罗汉果苷III为0％，罗汉果苷IIe为0％，蔗糖、果糖、葡萄糖、甘露醇皆为0％。该复配甜味剂中有杂味及有苦味的罗汉果总苷III及罗汉果总苷II的含量基本为0，且不含单糖与双糖等有能量的糖分，具有甜度高，甜味纯正，无杂味，超低热量的特点。
在一些优选的实施方式中，复配甜味剂是组分A，且其中含有47％到54％罗汉果苷V，1％到1.6％罗汉果苷VI，5％到8％11-O-罗汉果苷V，2.5％到4％异罗汉果苷V，1.5到2％赛门苷I，0.5％到2％罗汉果苷IVa，1％到2％罗汉果苷IVe，罗汉果苷III≤0.2％，罗汉果苷IIe为0％，0.1％到1％蔗糖，0.1％到1％果糖，0.1％到1％葡萄糖，0.1％到1％甘露醇。该复配甜味剂中仍然含有微量的罗汉果总苷III及罗汉果总苷II，因此保留少量的蔗糖、果糖、葡萄糖、甘露醇等糖类物质能增强复配甜味剂的前甜感，能够降低杂味，让口感更加接近蔗糖。
在一些优选的实施方式中，复配甜味剂是组分A，且其中含有23％到28％罗汉果苷V，0.2％到0.6％罗汉果苷VI，2％到4％11-O-罗汉果苷V，1％到2％异罗汉果苷V，0.3到1％赛门苷I，0.5％到1％罗汉果苷IVa，0.5％到1％罗汉果苷IVe，罗汉果苷III≤0.5％，罗汉果苷IIe≤0.1％，2％到6％蔗糖，2％到4％果糖，1％到4％葡萄糖，1％到4％甘露醇。该复配甜味剂中仍然含有少量的罗汉果总苷III及罗汉果总苷II，因此保留适当量的蔗糖、果糖、葡萄糖、甘露醇等罗汉果原料中本身含有的糖类物质能让复配 甜味剂的前甜感更强烈，能够起到适当降低苦味，掩盖杂味，让口感更加接近蔗糖的作用。
在本发明优选的实施方式中，该甜味制剂可以以粉末形式存在，且粉末的堆积密度(松密度)为20g/100ml至50g/100ml，在这样的堆积密度范围内，甜味制剂粉末能迅速溶解在水中，1g只需要30-50秒便能完全溶解到100ml常温的水中。粉末按照甜味组合物中罗汉果苷V含量的低到高，颜色从黄色到浅黄色，再到类白色，最后到纯白色。其中，该罗汉果甜味组合物也可以以液体形式存在，液体按照甜味组合物中罗汉果苷V含量的低到高，颜色从棕色到黄色，再到浅黄色，最后到无色。优选地是，该罗汉果甜味组合物以60-70Brix的水溶液形式存在。该甜味组合物也可以以无规则固体形式存在，优选地，以内部蓬松固体形式存在。
本领域技术人员可以根据需要将上述复配甜味剂加入食品、饮品、保健品、日化用品或药品中。
即本发明的第三目的在于提供了含有上述的甜味组合物的食品、饮品、保健品、日化用品、药品等。
本发明通过特定的制备方法有效地控制罗汉果苷III、IIe等含量，使得罗汉果甜味组合物的味道更好，且本发明的甜味组合物的制备过程中只用到纯水、不使用乙醇等有机溶剂，生产过程更加绿色健康。
附图说明
图1为对比例1所得粉末的HPLC图谱；
图2为实施例1所得的甜味组合物HPLC图谱；
图3为实施例2所得的甜味组合物HPLC图谱；
图4为实施例3所得的甜味组合物HPLC图谱；
图5为实施例2所得的甜味组合物与对比例1所得的粉末HPLC图谱。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步详细描述。以下 实施例用于说明本发明，但不用来限制本发明的范围。
实施例1
本实施例提供了一种从罗汉果中制备罗汉果甜味组合物的方法，具体包括如下步骤：
1)催熟：挑选熟透了的外表金黄色罗汉果300kg与1200kg青罗汉果(果龄为3个月以上)按照重量1：4交叉排列放置，保证成熟罗汉果释放的乙烯能与青罗汉果充分接触，上面覆盖塑料薄膜将罗汉果与外界空气隔开，起到维持乙烯高浓度与保温的作用，温度在25至38℃范围内催熟3天后，除掉覆盖的塑料薄膜，通风优良室温条件下再次催熟3天，挑选新的外表金黄色的罗汉果催熟下一批，极少量没有成熟的青果选入下一批被催熟，剩余的1200kg送往榨汁工序。
2)榨汁：使用挤压式榨汁机对罗汉果进行榨汁，保证罗汉果果籽的完整性，得到410kg的糖度为16Brix的果汁送往陶瓷膜过滤，机械方式对所得果渣饼进行分散，防止结块。
3)提取：分散的790kg果渣送入以下组合设备中：连续逆流提取机组A串联上榨汁机A，后面再串联连续逆流提取机组B，再串联榨汁机B。让果渣得以逆流提取，然后榨汁，再逆流提取，最后榨汁得到没有甜味的罗汉果废渣。提取温度为50℃，果渣与纯水接触的提取时间为20分钟，提取所用纯水量为790L。
4)离心：罗汉果挤压榨汁所得的果汁及提取液用卧螺离心机离心，转速3000r/min，转鼓内径为400mm。
5)过滤：离心液用孔径为50nm的陶瓷膜进行过滤，待过滤的液体温度控制在50℃以下。
6)吸附杂质：滤液以2BV/h的流速通过不锈钢层析柱，层析柱中装有400L型号为D101的非极性大孔吸附树脂，上柱的滤液温度为40℃左右。开始上柱的时候，罗汉果苷V、11-O-罗汉果苷V、赛门苷I等甜味成分会被吸附在树脂中，从层析柱中流出的液体主要是糖类、有机酸、无 机盐、氨基酸等成分，这些流出液可加工成糖浆做为其他商品。当罗汉果苷V开始泄露、出现在流出液中时，收集流出液，至滤液完全经过层析柱，并用450L左右纯水洗层析柱，收集并合并流出液，共1200L。
这些流出液以0.5BV/h的流速通过不锈钢层析柱，层析柱中装有1200L目数为80，型号为LX-17的极性大孔吸附树脂，以300L为一段，分部收集极性大孔树脂层析柱的流出液，共4段。上柱完成后，用纯水以1BV/h的流速洗2400L，以300L为一段，分部收集水洗液，共8段。按照收集的先后顺序，将流出液与水洗液命名为第1段、第2段、以此类推至第12段。第1、2段里面没有罗汉果甜苷含量，主要成分是单糖、双糖等可以浓缩成糖浆作为其他商品。合并第7、8、9段，共900L。
7)纳滤：合并的900L液体，用孔径为1nm的陶瓷膜进行纳滤。浓缩至截留液为100L左右，加入200L纯水稀释，继续纳滤浓缩至100L左右，如此稀释然后浓缩的过程再重复3次后，得100L无色透明液体。
8)浓缩干燥：100L液体继续使用多功能真空浓缩罐，温度65℃左右，真空度-0.08MPa左右，浓缩至进料固形物含量为30％，雾化器转速为20000r/min，进风温度180℃，出风温度95℃，得到堆积密度(松密度)为26g/100ml，规格为80％罗汉果苷V的纯白色罗汉果甜味组合物粉末，即甜味组合物。
步骤6)吸附杂质过程中中剩余的第3-6段与第10-12段合并共2100L，送纳滤工序然后浓缩干燥后可得到35％左右罗汉果苷V产品，也可以每段分开经过纳滤、浓缩、干燥得到10％至65％的罗汉果苷V的不同规格的产品。也可以这些段合并之后加入下一批重新上极性树脂柱以获得更高含量的产品。
实施例2
本实施例提供了一种从罗汉果中制备罗汉果甜味组合物的方法，具体包括如下步骤：
1)催熟：挑选熟透了的外表金黄色罗汉果250kg与1000kg青罗汉果 (果龄为3个月以上)按照重量1：4交叉排列放置，保证成熟罗汉果释放的乙烯能与青罗汉果充分接触，上面覆盖塑料薄膜将罗汉果与外界空气隔开，起到维持乙烯高浓度与保温的作用，温度在25至38℃范围内催熟2天后，除掉覆盖的塑料薄膜，通风优良室温条件下再次催熟2天，挑选新的外表金黄色的罗汉果催熟下一批，极少量没有成熟的青果选入下一批被催熟，剩余的1000kg送往榨汁工序。
2)榨汁：使用挤压式榨汁机对罗汉果进行榨汁，保证罗汉果果籽的完整性，得到350kg的糖度为17Brix的果汁送往陶瓷膜过滤，机械方式对所得果渣饼进行分散，防止结块。
3)提取：分散的650kg果渣送入连续逆流提取机组，果渣与纯水接触的提取时间为40分钟，提取过程所用纯水为650L。提取温度在70℃，提取液用板框热交换器冷却至50℃以下。
4)离心：罗汉果挤压榨汁所得的果汁及提取液用卧螺离心机离心，转速2500r/min，转鼓内径为400mm。
5)过滤：离心液用孔径为50nm的陶瓷膜进行过滤，待过滤的液体温度控制在50℃以下。
6)吸附杂质：滤液以1.5BV/h的流速通过不锈钢层析柱，层析柱中装有300L型号为HPD-722的弱极性大孔吸附树脂，上柱的滤液温度为40℃左右。开始上柱的时候，罗汉果苷V、11-O-罗汉果苷V、赛门苷I等甜味成分会被吸附在树脂中，从层析柱中流出的液体主要是糖类、有机酸、无机盐、氨基酸等成分，这些流出液可加工成糖浆做为其他商品。当罗汉果苷V开始泄露、出现在流出液中时，收集流出液，至滤液完全经过层析柱，并用450L左右纯水洗层析柱，收集并合并流出液，共1050L。
这些流出液以1BV/h的流速通过不锈钢层析柱，层析柱中装有1000L目数为60，型号为LX-17的极性大孔吸附树脂，流出液的前1000L里面没有罗汉果甜苷含量，主要成分是单糖、双糖等可以浓缩成糖浆作为其他商品。收集流出液的最后的400L。上柱完成后，用纯水以2BV/h的流 速洗2000L收集水洗液，合并最后的400L流出液与全部的水洗液，共2400L。
7)纳滤：上述合并的2400L液体，用孔径为2nm的陶瓷膜进行纳滤。浓缩至截留液为100L左右，加入200L纯水稀释，继续纳滤浓缩至100L左右，如此稀释然后浓缩的过程再重复2次后，得100L微黄色透明液体。
8)浓缩干燥：100L液体继续使用多功能真空浓缩罐，温度65℃左右，真空度-0.08MPa左右，浓缩至进料固形物含量为30％，雾化器转速为18000r/min，进风温度180℃，出风温度95℃，得到堆积密度(松密度)为33g/100ml，规格为50％罗汉果苷V的类白色罗汉果甜味组合物粉末。
实施例3
本实施例提供了一种从罗汉果中制备罗汉果甜味组合物的方法，具体包括如下步骤：
1)催熟：挑选熟透了的外表金黄色罗汉果320kg与1600kg青罗汉果(果龄为3个月以上)按照重量1：5交叉排列放置，保证成熟罗汉果释放的乙烯能与青罗汉果充分接触，上面覆盖塑料薄膜将罗汉果与外界空气隔开，起到维持乙烯高浓度与保温的作用，温度在25至38℃范围内催熟3天后，除掉覆盖的塑料薄膜，通风优良室温条件下再次催熟1天，挑选新的外表金黄色的罗汉果催熟下一批，极少量没有成熟的青果选入下一批被催熟，剩余的1600kg送往榨汁工序。
2)榨汁：使用挤压式榨汁机对罗汉果进行榨汁，保证罗汉果果籽的完整性，得到550kg的糖度为15Brix的果汁送往陶瓷膜过滤，机械方式对所得果渣饼进行分散，防止结块。
3)提取：1050kg分散的果渣用多功能提取罐进行提取，提取3次，第一次提取1.5h，提取温度100℃，第二次与第三次提取时间都为1h，温度都80℃，每次的提取所用纯水量都为2100L。提取液在提取罐底部得到200目钢筛过滤，合并三次提取液共5700L，并经过板框热交换器冷却至50℃左右送往离心工序。
4)离心：罗汉果挤压榨汁所得的果汁及提取液用卧螺离心机离心，转速2000r/min，转鼓内径为400mm。
5)过滤：离心液用孔径为100nm的陶瓷膜进行过滤，待过滤的液体温度控制在50℃以下。
6)吸附杂质：滤液以3BV/h的流速通过不锈钢层析柱，层析柱中装有400L型号为LX-60的非极性大孔吸附树脂，上柱的滤液温度为45℃左右。开始上柱的时候，罗汉果苷V、11-O-罗汉果苷V、赛门苷I等甜味成分会被吸附在树脂中，从层析柱中流出的液体主要是糖类、有机酸、无机盐、氨基酸等成分，这些流出液可加工成糖浆做为其他商品。当罗汉果苷V开始泄露、出现在流出液中时，收集流出液，至滤液完全经过层析柱，并用450L左右纯水洗层析柱，收集并合并流出液，共5400L。
这些流出液以2BV/h的流速通过不锈钢层析柱，层析柱中装有900L型号为LX-17的极性大孔吸附树脂，流出液的前1800L里面没有罗汉果甜苷含量，主要成分是单糖、双糖等，可以浓缩成糖浆作为其他商品。收集后续3600L流出液。上柱完成后，用纯水以2BV/h的流速洗1200L，并收集水洗液，合并收集的3600L流出液与1200L水洗液，共4800L。
7)纳滤：上述合并的4800L液体，用孔径为2nm的陶瓷膜进行纳滤。浓缩至截留液为200L左右，加入400L纯水稀释，继续纳滤浓缩至200L左右，如此稀释然后浓缩的过程再重复1次后，得200L黄色透明液体。
8)浓缩干燥：200L液体继续使用多功能真空浓缩罐，温度65℃左右，真空度-0.08MPa左右，浓缩至进料固形物含量为30％，雾化器转速为16000r/min，进风温度180℃，出风温度95℃，得到堆积密度(松密度)为42g/100ml，规格为25％罗汉果苷V的浅黄色罗汉果甜味组合物粉末。
对比例1
按照CN101522058A实施例1专利描述的方法，用罗汉果鲜果制备罗汉果三萜苷，得到微黄色粉末。
将实施例1、2、3与对比例1所得粉末用中国药典2015版中HPLC 检测罗汉果苷V方法：乙腈-水(23∶77)为流动相，检测波长为203nm，柱温30℃，流速：1ml/min，进样量：10ul，色谱柱：C18柱(4.6mm*150mm，5um)测得罗汉果苷VI，11-O-罗汉果苷V，罗汉果苷V，异罗汉果苷V，赛门苷I，罗汉果苷IVa，罗汉果苷IVe，罗汉果苷III，罗汉果苷IIe含量。
将实施例1、2、3与对比例1所得粉末使用离子色谱分析法(AOAC995.13)检测蔗糖、果糖、葡萄糖与甘露醇含量。
将实施例1、2、3与对比例1所得粉末，加入纯水，配置得到罗汉果苷V浓度(罗汉果苷V浓度为0.5mg/ml)相同的溶液，由20人(10男10女，年龄段20-61)组成的后苦味品尝小组，对以上4个不同溶液进行盲测，然后进行打分，品尝方法为先用纯水漱口，然后将需要品尝的溶液与舌头及口腔充分接触10s，然后吞咽(方便舌根深处能接触到溶液)，然后进行打分，在进行下次品尝前需漱口，前后两次品尝需要间隔至少1分钟。打分标准为后苦味越淡得分越高，后苦味越浓得分越低：无苦味(10分)，苦味不明显(9分、8分、7分，根据微苦的程度不同，分值也不同)，微苦(6分，5分，4分)，较苦(3分，2分，1分)。
结果如下表所示：
表1.实施例与对比例含量结果表
项目 实施例1 实施例2 实施例3 对比例1
罗汉果苷VI(％w/w) 0.59 1.48 0.45 1.22
11-O-罗汉果苷V(％w/w) 11.34 6.22 3.15 5.80
罗汉果苷V(％w/w) 80.62 53.61 27.14 48.20
异罗汉果苷V(％w/w) 3.69 3.42 1.62 2.53
赛门苷I(％w/w) 2.24 1.71 0.63 2.60
罗汉果苷IVa(％w/w) 0.21 0.63 0.83 2.25
罗汉果苷IVe(％w/w) 0.56 1.37 0.82 2.04
罗汉果苷III(％w/w) 0 0.13 0.35 1.52
罗汉果苷IIe(％w/w) 0 0 0 0.32
蔗糖(％w/w) 0 0.4 3.2 0
果糖(％w/w) 0 0.2 2.5 0
葡萄糖(％w/w) 0 0.2 1.4 0
甘露醇(％w/w) 0 0.5 1.6 0
口感评价得分 9.5 8.3 6.1 5.8
从表1、图1到5中可以得出，1、实施例2、3中所得罗汉果甜味组合物中含有蔗糖、果糖、葡萄糖、甘露醇这些糖类，实施例1没有，罗汉果苷V的含量越高，糖类的含量越低，低到为0％。而对比例中的罗汉果苷V含量与实施例2相近，但是不含有上述的这些糖类。10-60％左右的罗汉果苷V产品中带有少量单糖与双糖能起到丰富甜感，让滋味更加接近蔗糖的作用；2、所有实施例中都不含有罗汉果苷IIe，且罗汉果苷V的含量越高，罗汉果苷III的含量越小。实施例1得到的80.62％这样高含量的规格产品中，罗汉果苷III含量为0％，且其图谱中看不到罗汉果苷IIIe、罗汉果苷IIIa1的峰，这些味道不好甚至有强烈苦味的物质越少，口感评价的得分越高；3、实施例2与对比例1中罗汉果苷V的含量相近，实施例2中的极性比罗汉果苷V弱一些的赛门苷I、罗汉果苷IVa，罗汉果苷IVe的含量比对比例1低，且不含有极性比罗汉果苷IV更弱的罗汉果苷III、罗汉果苷IIe，而对比例1中含有，图5中实施例2的罗汉果苷IIIa1的峰值也比对比例1低，因此可以看出本方法通过对原料进行催熟，降低了苦味苷及味道不好的苷的含量，促进其转化成罗汉果甜苷，且后续的吸附杂质过程中，对罗汉果苷V吸附饱和的非极性或者弱极性树脂能显著吸附罗汉果总苷III及罗汉果总苷II，降低甚至除去味道不好的成分，提高产品的口感，但是该方法同时还能吸附部分的罗汉果总苷IV(赛门苷I、罗汉果苷IVa，罗汉果苷IVe等)可以通过后续的工艺改进将苦味苷与罗汉果总苷IV分离，从而开发新产品。
最后，本发明的方法仅为较佳的实施方案，并非用于限定本发明的保护范围。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
工业实用性
本发明提供一种从罗汉果中制备罗汉果甜味组合物的方法及其应用。本发明提供的从罗汉果中提取甜味组合物的方法优选包括如下步骤：对未成熟的罗汉果进行催熟，通过榨汁、纯水提取，去除杂质，浓缩纯化等步骤得甜味组合物。本发明还提供了含有上述甜味组合物的复配甜味剂，该复配甜味剂可广泛应用于食品、饮品、保健品、日化用品中。本发明通过控制罗汉果苷III、罗汉果苷IIe等含量，使得罗汉果甜味组合物的味道更好，且本发明的甜味组合物的制备过程中只用到纯水、不使用乙醇等有机溶剂，生产过程更加绿色健康，具有较好的经济价值和应用前景。

Claims (10)

  1. 一种从罗汉果中提取甜味组合物的方法，其特征在于，包括如下步骤：
    将成熟的罗汉果与未成熟的罗汉果按重量比为1:4～1:8放置在一起，在25～38℃下密封2～4天，再将其置于通风环境下1～4天得到罗汉果原料，将所述罗汉果原料榨汁得汁夜和果渣，合并所述汁液和使用纯水提取所述果渣后的提取液，除杂，浓缩纯化，即得。
  2. 根据权利要求1所述的方法，其特征在于，所述罗汉果为罗汉果亚属、无鳞罗汉果亚属、多倍体罗汉果或无籽罗汉果，优选为青皮果、长滩果或三倍体无籽罗汉果，进一步优选为有机青皮果、有机长滩果或有机三倍体无籽罗汉果。
  3. 根据权利要求1或2所述的方法，其特征在于，所述提取为连续逆流法或提取罐提取；
    所述连续逆流法优选具体包括如下步骤：以水为溶剂进行连续逆流法，所述果渣与水的用量比为1:1～1:2，提取温度为50～90℃，提取时间为30～40min；优选地，所述果渣与水的用量比为1:1，提取温度为50℃，所述果渣与水的接触时间为15～30min；
    和/或，在所述连续逆流法中，优选采用两台连续逆流提取机串联，每台逆流提取机组再串联两台挤压榨汁机，以合并所述汁液和提取液。
  4. 根据权利要求1至3中任一项所述的方法，其特征在于，所述除杂具体包括如下步骤：a)离心去除所述提取液中果肉组织；b)将离心液使用孔径为50～100nm的陶瓷膜过滤得滤液；c)使用大孔吸附树脂层析柱吸附所述滤液中的杂质。
  5. 根据权利要求4所述的方法，其特征在于，所述“使用大孔吸附树脂层析柱吸附所述滤液中的杂质”具体包括如下步骤：
    1)使用非极性大孔吸附树脂层析柱或者弱极性大孔吸附树脂层析柱吸附滤液中极性比罗汉果主要甜味成分弱的物质，从有罗汉果苷V有泄露时开始收集流出液；
    2)使用极性大孔吸附树脂层析柱吸附步骤1)中收集的流出液中的杂质多酚和有机酸，分部收集流出液；
    3)用纯水洗步骤2)中的层析柱，分部收集水洗液，选择性地合并水洗液与步骤2)中分部收集的流出液，取口感好的组分浓缩纯化，舍去口感不好的组分。
  6. 根据权利要求5所述的方法，其特征在于，所述非极性大孔吸附树脂优选型号为D101和/或LX-60；所述弱极性大孔吸附树脂优选型号为HPD-722和/或AB-8；所述极性大孔树脂优选型号为LX-17，更加优选地为60-120目数的LX-17；
    所述非极性大孔吸附树脂柱中的树脂用量与所述罗汉果总量的体积质量比(L/kg)优选为1:2～1:5，流速优选为1～3BV/h；
    所述极性大孔吸附树脂柱中的树脂用量与上柱液中罗汉果苷V的体积质量比(L/kg)优选为50:1～200:1。
  7. 根据权利要求1至6中任一项所述的方法，其特征在于，所述“浓缩纯化”具体包括如下步骤：使用孔径为1～2nm的纳滤膜浓缩纯化去除杂质后的溶液；所述纳滤膜的材质优选为醋酸纤维素、磺化聚砜、磺化聚醚砜、聚乙烯醇、聚酰胺、陶瓷或金属，进一步优选为陶瓷。
  8. 一种罗汉果甜味组合物，其特征在于，包括如下组分：10％到85％罗汉果苷V，0.2％到2％罗汉果苷VI，1％到12％11-O-罗汉果苷V，0.5％到5％异罗汉果苷V，0.1％到3％赛门苷I，0.1％到3％罗汉果苷IVa，0.2％到3％罗汉果苷IVe，0％到12％蔗糖，0％到8％果糖，0％到6％葡萄糖和0％到10％甘露醇，且罗汉果苷III≤0.5％，罗汉果苷IIe≤0.1％。
  9. 一种复配甜味制剂，其特征在于，包括权利要求1至9中任一项所述的方法提取得到的甜味组合物和/或添加剂，所述添加剂为甜味剂、香精香料、调味剂、色素、植物提取物、赋形剂中的一种或多种。
  10. 含有权利要求9所述的复配甜味制剂的食品、饮品、保健品、日化用品或药品。
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