WO2021027056A1 - 罗汉果苷甜味和风味组合物及其制备方法与应用 - Google Patents

罗汉果苷甜味和风味组合物及其制备方法与应用 Download PDF

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WO2021027056A1
WO2021027056A1 PCT/CN2019/111855 CN2019111855W WO2021027056A1 WO 2021027056 A1 WO2021027056 A1 WO 2021027056A1 CN 2019111855 W CN2019111855 W CN 2019111855W WO 2021027056 A1 WO2021027056 A1 WO 2021027056A1
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resin
membrane
extraction
mogroside
han guo
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French (fr)
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黄华学
刘庚贵
刘永胜
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湖南艾达伦科技有限公司
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • A23L2/08Concentrating or drying of juices
    • A23L2/082Concentrating or drying of juices by membrane processes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385Concentrates of non-alcoholic beverages
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/72Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration
    • A23L2/74Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by filtration using membranes, e.g. osmosis, ultrafiltration
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/80Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by adsorption
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/10Natural spices, flavouring agents or condiments; Extracts thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/30Artificial sweetening agents
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115Fatty acids or derivatives thereof; Fats or oils
    • A23L33/12Fatty acids or derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/42Cucurbitaceae (Cucumber family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • A61P11/10Expectorants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00Drugs for disorders of the respiratory system
    • A61P11/14Antitussive agents
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

Definitions

  • the present invention relates to a mogroside sweetness and flavor composition and a preparation method thereof, and the application of the composition, in particular to a mogroside aromatic volatile oil, sweet flavor decolorizing concentrated juice, pure flavor decolorizing concentrated juice and mogroside sweetening Mogroside sweetness and flavor composition composed of flavor components, and a method for extracting mogroside aromatic volatile oil, sweet flavor decolorizing concentrated juice, pure decolorizing concentrated juice and mogroside sweetening components by using fresh Luo Han Guo or seedless Luo Han Guo as raw materials , And the application of the mogroside sweetness and flavor composition in foods, beverages, dairy products, health care products and medicines.
  • Luo Han Guo (Siraitia grosvenorii (Swingle) C. Jeffrey), English name: fructus momordicae, is the fruit of perennial vines in the Cucurbitaceae family. Also known as Lahan fruit, fake bitter gourd, light fruit mussel, Jinbuhuan, Luohanbiao, naked tortoise shell, it is known as "fairy fruit", its leaves are heart-shaped, dioecious, bloom in summer, and bear fruit in autumn.
  • Seedless momordica grosvenoris is a system of planting triploid plants and diploid male plants of momordica grosvenori. When flowering, the triploid female plants are artificially pollinated with diploid male plants, and the female plants bear fruit to obtain seedless momordica grosvenori.
  • Momordica grosvenori and seedless Momordica grosvenori are rich in flavor and nutrients, as well as non-sugar sweetness components of triterpene saponins.
  • Luo Han Guo fruit contains 0.2% to 0.3% of volatile oil. There are more than 20 volatile oil components. 13 main components have been identified: undecyl alcohol, cooperanol, butylphenol ketone, T-orsophorol, 1-naphthol, 1,2,3,4,4a,7,8,8a,-octahydro-1,6 dimethyl-4-(1-methylethyl)-cedarol, tridecyl cyclopropanoate, ten Pentadecanoic acid, n-heptadecanol, methyl hexadecanoate, n-hexadecanoic acid, methyl 9,12-octadecadienoate, 9,12-octadecadienoic acid, It accounts for 94.96% of the total volatile oil. Among them, n-hexadecanoic acid (45.609%) and 9,12-octadecadienoic acid (36.151%) are the main components, which together
  • the composition of the volatile oil of the seedless Luo Han Guo is similar to that of Luo Han Guo, but the content has changed. At present, 24 components have been identified. Including: ethylene glycol isopropyl ether (27.21%), 1,2-butyl-2-ethylhexyl phthalate (13.51%), diisobutyl phthalate (10.85%), geranium aldehyde (10.22%), (E) 3-decenoic acid (6.52%), butyl butyrate (4.99%), 2-tridecyl acetate (4.86%), which together accounted for 78.16% of the total volatile oil.
  • Momordica grosvenori and seedless Momordica grosvenori both contain triterpene saponins of Momordica grosvenori, glucose (glucose), fructose (fructose) accounted for 14%, more than ten kinds of essential amino acids, protein, fatty acids, flavonoids, vitamin C and manganese, iron, nickel , Selenium, tin, iodine, molybdenum and other 26 kinds of inorganic elements and trace elements.
  • Cucurbitacin triterpenes These compounds are the main active ingredients in Luo Han Guo, and they have a common aglycon structure. These substances in Luo Han Guo are sweet substances or slightly sweet substances except for a few. Among them, mogroside V is the main sweet ingredient. It is non-toxic, low-calorie, high sweetness, and good thermal stability. It is a natural sweetener substance.
  • Protein and amino acid The dried fruit of Luo Han Guo contains 7.1%-7.8% protein. In its hydrolysate, except tryptophan has not been determined, 18 kinds of amino acids are complete. Among the determined amino acids, the higher content is glutamic acid (108.2-113.3mg/kg), aspartic acid (93.9-112.5mg/kg), valine (52.5-55.5mg/kg), alanine Acid (49.9-66.8mg/kg), Leucine (48.5-56.7mg/kg). Glutamic acid is the largest non-essential amino acid in the human body and an important raw material for the synthesis of glutathione. It can be seen that Luo Han Guo has high nutritional value.
  • Luo Han Guo fruit contains 24 kinds of inorganic elements, of which 16 are essential trace elements and a wide range of elements for the human body.
  • the elements with higher content are potassium (12290mg/kg), calcium (667mg/kg), magnesium (550mg/kg) ).
  • the selenium contained in Luo Han Guo reaches 0.186 mg/kg, which is 2 to 4 times that of grains. Elemental selenium has a good effect in the prevention and treatment of coronary heart disease, anti-aging and anti-cancer.
  • Luo Han Guo fruit contains non-sugar sweet components, mainly triterpene saponins: mogroside (mogroside) V and IV.
  • mogroside V is 256-344 times that of srcrose
  • mogroside IV is 126 times that of sucrose
  • the second is D-mannitol, whose sweetness is 0.55 of that of sucrose. -0.65 times.
  • the main sweet component in Luo Han Guo is a type of saponins with mogroside alcohol, a cucurbitacin triterpene, as aglycon. These saponins are sweet saponins (containing 4 or more glucose groups) and tasteless or Saponins with peculiar and bitter taste (containing 3 or less glucose groups).
  • the sweet mogrosides include 11-O-mogroside V, new mogroside, mogroside V, isomogroside V, simenoside I, mogroside VI, mogroside IVe, mogroside IVa, etc.; there is 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 IIe, etc.) Glycosides IIb, 11-O-mogroside IIe, etc.), mogroside total I (including mogroside Ia1, mogroside Ie1, etc.).
  • Luo Han Guo and Seedless Luo Han Guo at home and abroad there is a lot of research on Luo Han Guo and Seedless Luo Han Guo at home and abroad, and there are also various specifications of Luo Han Guo extracts on the market.
  • the focus of the research is the separation and purification of mogroside saponins and mogroside juice concentrate, and the mogroside extracts sold on the market are mainly ordinary mogroside juice concentrates and powdered specifications with a content of 20% to 60% mogroside V.
  • the technical solutions disclosed in CN201810969469, CN201810320300, CN201710743703, CN201710469860, CN201710277285, CN201210207266, CN200810097509, etc. are all based on the extraction of Luo Han Guo concentrated juice.
  • the Luo Han Guo concentrated juice produced by this kind of technology does not collect the aromatic volatile oil of Luo Han Guo, and a large amount of the aromatic volatile oil of Luo Han Guo is lost in the production process.
  • Luo Han Guo concentrated juice has neither the aromatic taste of roasted Luo Han Guo nor the burnt aroma of peeled and dried Luo Han Guo, so that the flavor is lacking and the taste is slightly worse.
  • the technical solutions disclosed in CN201811397385, CN201811250821, CN201711214793, CN201710388435, CN201610387839, CN02128065, etc. are all based on the purification of mogroside V.
  • the Momordica grosvenori extract produced by this kind of technology is mainly based on the extraction of the sweetness components of Momordica grosvenori saponins, which completely removes the flavor and nutrients of Momordica grosvenori, and is only used as a sweetener. And because the sweetness components are relatively pure, the sweetness lasts for a long time, which is not acceptable to all people, and it is not a flavored and nutritious Luo Han Guo extract.
  • the technical problem to be solved by the present invention is to overcome the above-mentioned shortcomings in the prior art and provide a mogroside sweetness and flavor composition, which does not contain bitter substances, but retains the unique flavor and nutritional components of mogroside.
  • the peculiar fruity aroma and burnt aroma of the rich Luo Han Guo has a refreshing sweetness and pure taste close to that of sucrose. The sweetness lasts for a short time. It integrates the aroma, sweetness, taste and nutrients of Luo Han Guo.
  • the further technical problem to be solved by the present invention is to provide a method for preparing the mogroside mogroside aromatic volatile oil, sweet flavor decolorizing concentrated juice, pure flavor decolorizing concentrated juice, and mogroside sweet components.
  • a mogroside sweetness and flavor composition comprising at least one of mogroside aromatic volatile oil, sweet decolorization concentrated juice, pure decolorization concentrated juice, and mogroside sweetness components Species, of which sweet flavor decolorized concentrated juice, pure flavor decolorized concentrated juice and mogroside sweetness component ⁇ 0.
  • the mass content of mogroside V is 1%-15%.
  • the composition contains n-hexadecanoic acid or/and 9,12-octadecadienoic acid, which is a volatile oil component of Luo Han Guo, or ethylene glycol isopropyl ether and 1,2-benzene
  • n-hexadecanoic acid or/and 9,12-octadecadienoic acid which is a volatile oil component of Luo Han Guo, or ethylene glycol isopropyl ether and 1,2-benzene
  • One of butyl-2-ethylhexyl dicarboxylate, diisobutyl phthalate, geranium aldehyde, or a combination of several components of the volatile oil of Luo Han Guo, and the total mass content of the volatile oil is 0% to 5%; preferably 0.5% to 4.0%.
  • the technical solution adopted by the present invention to further solve its technical problems is a preparation method of mogroside sweetness and flavor composition, including the following steps: (I) collection of mogroside aromatic volatile oil; (II) extraction of mogroside sweet flavor decolorized concentrated juice Refining; (III) Extraction and refining of Luohanguo pure decolorizing concentrated juice; (IV) Extraction and refining of mogroside sweet components; (V) Mixing.
  • step (I) the method for collecting the aromatic volatile oil of Luo Han Guo is:
  • Optimal plan Use the Momordica grosvenori special measuring board to classify fresh Momordica grosvenori according to large, medium, small and extrinsic fruits; then install them in a special basket for Momordica grosvenori according to the category; the number of layers is 2 to 4, and the number of days it is placed indoors It is 7 to 10 days, turning once every 3 to 4 days in the middle; until the surface of the fruit has ⁇ 50% of the area appearing yellow, the weight loss by water evaporation accounts for 10-15% of the fruit weight;
  • a further preferred solution use the dedicated fruit measuring board for Luo Han Guo to classify fresh Luo Han Guo according to large, medium, small and extrinsic fruits to improve classification efficiency;
  • step (1) Saccharification into net trays according to the large, medium, small, and outer fruit categories, and then place them in the fragrant volatile oil collection Place the net plate of the roasting room of the device on the rack, ignite and heat up and bake;
  • the aromatic volatile oil contained in Luo Han Guo will gradually volatilize and evaporate. After cooling, it will form a mixture of aromatic volatile oil and water, which will be collected by the aromatic volatile oil collection device in the roasting bar to obtain the aromatic volatile oil of Luo Han Guo; , Also got the dried fruit of Luo Han Guo;
  • the preferred baking method During the baking process, the heating and cooling process of baking is divided into the following three stages:
  • the first stage increase the temperature to 45°C ⁇ 50°C for 2 ⁇ 3 days, so that the water and aromatic volatile oil in Luo Han Guo will gradually be discharged, evaporated and volatilized;
  • the second stage gradually increase the temperature to 65°C ⁇ 70°C for 2 ⁇ 3 days to accelerate the discharge, evaporation and volatilization of water and aromatic volatile oil;
  • the third stage Cool down to 55°C ⁇ 60°C, continue baking, reduce the weight of the fruit to 25 ⁇ 30% of the fresh fruit, then stop the fire, naturally cool down to ambient temperature, and release;
  • the preferred scheme of the aromatic volatile oil collection device is composed of the following components: including a stainless steel pipe, the head end of the stainless steel pipe is connected with the exhaust hole on the top of the barn, and the tail end of the stainless steel pipe extends out of the barn and extends out of the barn.
  • the outside of the room is equipped with a cooling device on the outside of the pipe wall of the stainless steel pipe.
  • the end outlet of the stainless steel pipe is provided with an aromatic volatile oil collection and storage tank for receiving a mixture of aromatic volatile oil and water.
  • the side wall of the aromatic volatile oil collection and storage tank is provided for observation Collect the liquid level indicator of the liquid level in the storage tank.
  • the method for extracting and refining the sweet flavor decolorized concentrated juice includes the following steps: saccharification and ripening; peeling and baking in a special oven; extraction; centrifugal filtration and ceramic membrane clarification; membrane separation and concentration; resin decolorization ; Resin debittering, pesticide residue removal, heavy metal removal; activated carbon to remove peculiar smell; ceramic membrane clarification; vacuum concentration;
  • Saccharification post-cooking the operation method is the same as step (I) (1) Saccharification post-cooking;
  • the aromatic volatile oil contained in the peeled momordica grosvenori will gradually volatilize and evaporate along with the water at the same time. After cooling, a mixture of aromatic volatile oil and water is formed, which is collected by the set aromatic volatile oil collection device to obtain the aromatic volatile oil of momordica grosvenori;
  • Paving optimal plan According to the classification of large, medium, small and outer fruit, paving;
  • the preferred baking method During the baking process, the heating and cooling process of baking is divided into the following three stages:
  • the first stage Raise the temperature to 80°C ⁇ 85°C for 4 ⁇ 8h;
  • the second stage cooling to 75°C ⁇ 70°C for 16 ⁇ 24h;
  • the third stage Cool down to 65°C ⁇ 60°C, continue to bake for 30 ⁇ 40h, make the weight of the fruit drop to 20 ⁇ 30% of the weight of peeled fruit, the surface is dark yellow to yellowish brown, and has a strong fruit flavor
  • stop baking cool down naturally, and leave the box;
  • the preferred structure of the aromatic volatile oil collection device is composed of the following components: including a stainless steel pipe, the head of the stainless steel pipe is connected with the exhaust hole on the top of the oven, and the tail end of the stainless steel pipe extends out of the roasting barn
  • the outer stainless steel pipe has a cooling device on the outside of the pipe wall.
  • the end outlet of the stainless steel pipe is provided with an aromatic volatile oil collection and storage tank for receiving a mixture of aromatic volatile oil and water;
  • the sidewall of the aromatic volatile oil collection and storage tank is provided with a side wall for observation, collection and storage. Liquid level indicator of the liquid level in the tank;
  • the water is purified water; the extraction temperature is preferably 80°C to 95°C; the number of extractions is 3 times, and the extraction time is 1.5 to 2.5 hours, 1.0 to 2.0 hours, and 0.5 to 1.5 hours; each purified water is added The volume is 8-10 times, 7-9 times, 5-7 times the weight of the peeled Luo Han Guo dried fruit; after each extraction, filter, the filter residue enters the next extraction, after the third extraction is completed, the filter residue is processed separately; Combine the three extractions to obtain the extraction tank extract;
  • step (II) Counter-current extraction tank extraction: Put the peeled Luo Han Guo dried fruit obtained in step (2) of step (II) into a counter-current extraction tank, and add water for counter-current extraction;
  • the water is purified water; the extraction temperature is preferably 80°C to 95°C; the extraction time is 1.5-2.5h; the volume of purified water added is 4-6 times the weight of the peeled Luo Han Guo dried fruit (purified water volume/dry Peel and fruit, V/W); after the extraction is completed, filter, and the filter residue is treated separately; combine the continuously flowing extracts to obtain the countercurrent extraction tank extract;
  • Decanter centrifugation Filter the extraction tank extract or countercurrent extract through a decanter centrifuge to obtain the decanter centrifuge filtrate;
  • the ceramic membrane filtrate is cooled by water, and then the ultrafiltration membrane is used to separate most of the pigment through the membrane, and then concentrated with a reverse osmosis membrane to facilitate decolorization and subsequent operations;
  • Ultrafiltration decolorization Decolorize the cooled ceramic membrane filtrate through a complete set of ultrafiltration membrane equipment, select the ultrafiltration membrane with a pore size of 8KD ⁇ 10KD, collect the downstream liquid of the membrane, that is, the decolorization liquid, to obtain the membrane decolorization liquid;
  • Reverse osmosis membrane concentration the membrane decolorizing solution is concentrated to 5-10 Brix through the reverse osmosis membrane complete set of equipment to obtain membrane concentrate;
  • the anionic resin includes gel type and macroporous acrylic acid weak base anion resin, acrylic acid base and weak base anion resin, gel type and macroporous styrene base anion resin, macroporous acrylic acid Strong base anion resin, macroporous styrene weak base anion resin;
  • the cationic resin includes gel type and macroporous styrene strong acid cationic resin, acrylic gel type and macroporous weak acid cationic resin;
  • the preferred model of cationic resin 001 ⁇ 16, D717;
  • anionic resin 350kg-5500kg per 1000kg peeled Luo Han Guo dried fruit; decolor the membrane concentrate through an anionic resin. After feeding, wash the column with purified water to wash out the active ingredients remaining in the column; combine and flow out Liquid and washing liquid to obtain anionic resin decolorizing liquid;
  • the amount of cationic resin is: 250kg-450kg per 1000kg of peeled Luo Han Guo dried fruit; the anionic resin decolorizing solution is desalinated by the cationic resin, and after feeding, the column is washed with purified water to wash out the active ingredients remaining in the column; combine The effluent and the washing liquid are used to obtain the cationic resin desalting liquid;
  • the resins used for debittering, removing pesticide residues, and removing heavy metals include gel and macroporous acrylic resins, acrylic resins, gel and macroporous styrene resins, macroporous acrylic resins, and macroporous acrylic resins. Porous styrene resin, acrylic gel resin;
  • Preferred models of special resin for debittering LSA-600, LX-900;
  • the dosage is 250kg ⁇ 350kg per 1000kg of peeled Momordica grosvenori dried fruit; pass the cationic resin desalting solution through the special resin column for debittering to debitter, after feeding, wash the column with purified water to keep the remaining in the column The active ingredients are washed out. Combine the effluent and the washing liquid to obtain the debittering liquid;
  • the dosage is 250kg-350kg per 1000kg of peeled Luo Han Guo dried fruit; pass the debittering liquid through the special resin column for de-pesticide residue to remove the pesticide residue, and then wash the column with purified water after feeding. The remaining active ingredients are washed out; the effluent and the washing liquid are combined to obtain the debittering and de-pesticide residue liquid;
  • the dosage is 250kg ⁇ 350kg per 1000kg of peeled Luo Han Guo dried fruit; pass the debittering and agricultural residue removal through a special resin column for heavy metal removal to remove heavy metals. After feeding, wash the column with purified water to remove The remaining active ingredients are washed out; the effluent and the washing liquid are combined to obtain a debittering and de-pesticide-removing liquid for heavy metal removal;
  • the amount of activated carbon used is 12kg-20kg per 1000kg of peeled Luo Han Guo dried fruit; the activated carbon is granular activated carbon;
  • the preferred solution pre-load activated carbon in the chromatography column, then pass the debittering and de-pesticide residues and heavy metal removal liquid through the activated carbon column to remove odor. After the feed is completed, wash the column with purified water; combine the effluent and washing liquid, and filter by plate and frame , Get debittering, de-pesticide residue, heavy metal deodorizing liquid;
  • the method for extracting and refining the pure flavor decolorizing concentrated juice includes the following steps: using fresh and ripe Luo Han Guo as a raw material, saccharifying and ripening; then extracting with an extraction tank or a countercurrent extraction tank; centrifugal filtration and ceramics Membrane clarification; membrane separation and concentration; resin decolorization; resin debittering, pesticide residue removal, and heavy metal removal; activated carbon to remove peculiar smell; ceramic membrane clarification; vacuum concentration;
  • Extraction tank extraction The operation method is basically the same as step (II) (3) Sweet fragrant decolorizing concentrated juice A.
  • Extraction item a) Extraction tank extraction the difference is that the raw material here is fresh Luo Han Guo, and purified water is added The volume is 2 to 4 times, 2 to 4 times, and 2 to 3 times the mass of Luo Han Guo;
  • Counter-current extraction tank extraction The operation method is basically the same as step (II) (3) Sweet fragrant decolorizing concentrated juice A. Extraction b) Counter-current extraction tank extraction, the difference is that the volume of purified water added is the quality of fresh Luo Han Guo 1.2 ⁇ 2.0 times;
  • step (II) Sweet fragrant decolorizing concentrated juice D. Resin decolorization, the difference is that the more preferred solution:
  • Anion resin The amount of anion resin is 90kg ⁇ 150kg per 1000kg of anion resin for fresh Luo Han Guo;
  • Cationic resin The amount of cationic resin is 60kg ⁇ 120kg per 1000kg fresh Luohan;
  • step (II) sweet fragrant decolorizing concentrated juice E. Resin debittering, removal of pesticide residues, and removal of heavy metals, the difference is that a more preferred solution:
  • the operation method is basically the same as step (II) (3) Sweet fragrant decolorizing concentrated juice F. Activated carbon to remove peculiar smell, the difference is that the amount of activated carbon is 3-5kg per 1000kg of fresh Luo Han Guo;
  • step (II) sweet flavor decolorizing concentrated juice H. Vacuum concentration.
  • the method for extracting and refining the sweet components of mogroside includes the following steps: saccharification and ripening of fresh and mature mogroside, extraction in an extraction tank or countercurrent extraction tank, centrifugal filtration and ceramic membrane clarification, and membrane separation Refining, resin decolorization, resin debittering, pesticide residue, and heavy metal removal, activated carbon to remove pesticide residue and odor, ceramic membrane clarification, membrane separation and odor removal, vacuum concentration and drying;
  • step (III) centrifugal filtration and ceramic membrane clarification
  • the membrane is an ultrafiltration membrane; the ceramic membrane filtrate is cooled by passing water, and according to the difference in the molecular weight of the mogroside sweetness component, a large molecular weight ultrafiltration membrane is used for molecular retention to remove most of the pigments and impurities, and then a small molecular weight The ultrafiltration membrane is used for molecular retention to collect the sweet components of mogroside;
  • High molecular weight ultrafiltration refining the ceramic membrane filtrate cooled to below 45°C is refined through a complete set of large molecular weight ultrafiltration membrane equipment.
  • the pore size of the ultrafiltration membrane is 8KD ⁇ 10KD, and the downstream liquid of the membrane is collected to obtain the high molecular weight ultrafiltration membrane. Filter membrane refined liquid;
  • Small molecular weight ultrafiltration refining and concentration pass the high molecular weight ultrafiltration membrane refined liquid through a small molecular weight ultrafiltration membrane complete set of equipment to refine, select the ultrafiltration membrane pore size 2KD ⁇ 3KD, collect the upstream liquid of the membrane, namely the refined liquid, to obtain small molecular weight ultrafiltration Membrane refined liquid;
  • step (III) resin decolorization
  • step (III) resin debittering, pesticide residue removal, and heavy metal removal
  • step (III) activated carbon to remove peculiar smell
  • step (III) ceramic membrane clarification
  • the membrane is a nanofiltration membrane
  • the vacuum concentrate is spray-dried or microwave vacuum-dried to obtain the mogroside sweetness component product.
  • step (V) the compounding refers to combining the collected aromatic volatile oil of the roasted Luo Han Guo, the extracted and refined sweet flavor decolorizing concentrated juice, the pure flavor decolorizing concentrated juice, and the sweet components of mogroside according to the desired product taste, Smell, sweetness persistence, product existence form requirements, determine the specific proportion of each component, and mix.
  • the mogroside sweetness and flavor composition of the present invention can be widely used in the fields of food, beverages, dairy products, health care products, medicines and the like.
  • step (I) of the preparation method of the present invention with regard to the roasting of Luo Han Guo and the collection of aromatic volatile oil, the inventor’s research has shown that during the roasting process of Luo Han Guo, it emits the odor of the aromatic volatile oil of Luo Han Guo with a strong fruity and burnt aroma; Luo Han Guo concentrated juice or powdered Luo Han Guo extract does not have this special Luo Han Guo fruit aroma and burnt aroma. Therefore, the inventor designed a special device to collect the aromatic volatile oil during the baking process and add this volatile oil to the Luo Han Guo extract. To enhance the unique aroma of Luo Han Guo extract, improve the taste, and improve the quality of Luo Han Guo related products.
  • step (II) regarding the extraction and purification of sweet flavor decolorizing concentrated juice, the inventor’s research shows that the peeled and dried Luo Han Guo, that is, the peeled Luo Han Guo with a brown to brown surface, is particularly refreshing after making tea The sweetness, and restores the special fruit aroma and burnt aroma of Luo Han Guo. Therefore, the present inventor changed the previous process of directly extracting Luo Han Guo concentrated juice from fresh Luo Han Guo. First, the fresh Luo Han Guo was peeled and roasted, so that the fresh Luo Han Guo had a special sweet aroma and burnt aroma, as well as a pure sweet taste. Some extraction and separation processes produce decolorized concentrated juice with sweet flavor.
  • the inventor’s research also showed that it was discovered that during the roasting process of the peeled Luo Han Guo, the peculiar fruit aroma and burnt aroma of Luo Han Guo were also produced. Therefore, the volatile oil produced during the roasting process of the peeled Luo Han Guo was also collected. , In order to get all the effective active ingredients of Luo Han Guo as much as possible.
  • step (II) although the raw material is dried and peeled momordica grosvenori, the difference is that fresh momordica grosvenori is used as the raw material for crushing and extraction, but because the peel has been peeled during the preliminary drying process, and experiments have proved that the extraction method can completely remove The dry skin of Luo Han Guo is completely extracted.
  • the centrifugal filtration and ceramic membrane clarification are preferably performed by decanter centrifugal filtration, then disc centrifugal filtration, and finally ceramic membrane clarification. There is a corresponding order in use, and the effect is best. .
  • steps (II) to (IV) the ceramic membrane clarification is used twice, but the preferred ceramic membrane pore size is different, the first time is 0.45 ⁇ m, the second time is 0.22 ⁇ m, the purpose is to completely remove The fine particles are precipitated during the production process to obtain a completely clear and transparent product.
  • step (II) to (III) the membrane separation and concentration, it is preferable to use an ultrafiltration membrane with a pore size of 8KD ⁇ 10KD to separate and remove pigments and macromolecular impurities, and then concentrate through a reverse osmosis membrane to obtain a membrane with a corresponding concentration. Concentrate.
  • the membrane separation and refining process preferably uses an ultrafiltration membrane of 8KD-10KD to separate and remove pigments and macromolecular impurities.
  • the liquid downstream of the membrane, that is, the permeate, is collected;
  • the ultrafiltration membrane separates and removes components such as glucose, fructose, and amino acids, and collects the liquid upstream of the membrane, that is, the retentate. Because the average molecular weight of mogroside and other sweet components is about 1200, plus the molecular structure characteristics, selecting an ultrafiltration membrane in this range can obtain purified mogroside and other sweet components while removing most of the remaining impurities.
  • the activated carbon is granular activated carbon instead of powdered activated carbon.
  • the purpose of the granular activated carbon used is to improve the taste and remove a very small amount of pesticide residues, not for decolorization.
  • step (IV) the drying method is spray drying or microwave vacuum drying, and other drying methods have poor effect.
  • the content of mogroside V is preferably 1% to 15% (w/w).
  • the diluted or dissolved aqueous solution has a solid content of 1% w/v and the absorbance at 420 nm is ⁇ 0.5.
  • the content of mogroside V is determined by HPLC according to the standard of "Chinese Pharmacopoeia”.
  • composition of the present invention contains or does not contain n-hexadecanoic acid, 9,12-octadecadienoic acid and other volatile oil components of Momordica grosvenori, ethylene glycol isopropyl ether, 1,2-butyl-2-phthalate Ethylhexyl, diisobutyl phthalate, geranium aldehyde and other seedless Luo Han Guo volatile oil components and the combination of Luo Han Guo and seedless Luo Han Guo volatile oil components, the total volatile oil content is 0% to 5%, wherein the volatile oil content is based on the "
  • the Chinese Pharmacopoeia standard is determined by the volatile oil determination method, and the single component volatile oil content is determined by the GC method.
  • the present invention uses Luo Han Guo or/and seedless Luo Han Guo as raw materials.
  • Luo Han Guo and Seedless Luo Han Guo contain a variety of volatile oils and have special aromatic odors, but the aromatic and burnt aromas cannot be reflected in the fresh fruits. Only during and after baking can people smell them.
  • Aromatic and burnt aroma Therefore, we can collect the aromatic volatile oil of the roasted fruit and the peeled fruit during the roasting process of the Luo Han Guo and the seedless Luo Han Guo without increasing the cost, and then add it as a raw material to the composition of the present invention. Or for other purposes.
  • Luo Han Guo has a special sweet aroma after peeling and baking, and this taste can be well preserved under the process conditions of the present invention.
  • a sweet aroma can be obtained.
  • the decolorized juice concentrate is obtained.
  • the nutrients contained in Luo Han Guo and sweet components such as mogroside are easily soluble in water and can be extracted by water.
  • the water extract contains turbid substances and must be refined. For example, after two-stage centrifugation and ceramic membrane clarification, a clear and transparent liquid can be obtained, otherwise it is easy to block the ceramic membrane equipment.
  • a reverse osmosis membrane can be used to concentrate the aforementioned membrane decolorization liquid.
  • the anionic resin has a decolorizing effect on the decolorizing liquid of Momordica grosvenori after membrane separation and decolorization, and a specific type of anionic resin is preferred for better decolorization.
  • the anion resin exchange adsorption the pigment is adsorbed by the resin, while mogroside and other sweet substances and nutrients are not adsorbed and flow out.
  • the cationic resin is used to restore the pH value of the decolorizing liquid treated by the anion resin to the initial state, that is, the system is realized The acid-base reduction.
  • Luo Han Guo has a very small amount of bitter components, pesticide residues and heavy metals in its original state. These harmful substances will always exist in the process.
  • these substances must be removed to make the content of these substances in the product meet the standard.
  • the taste of the product is further improved by granular activated carbon, or the remaining pesticide residues are removed at the same time, so as to obtain nearly perfect sweet flavor decolorized concentrated juice and pure flavor decolorized concentrated juice.
  • the extracted sweet components such as mogroside exist in the form of powder, which is different from the sweet flavor decolorization concentrated juice and pure flavor decolorization concentrated juice in terms of technology. If the sweet flavor decolorized concentrated juice and pure flavor decolorized concentrated juice are directly dried, the expected drying purpose cannot be achieved because they contain a large amount of low-carbon sugars and other components, so these substances need to be removed.
  • the ultrafiltration membrane of appropriate specifications can retain the sweet components such as mogroside with an average molecular weight of about 1200, and remove low-carbon sugars and other substances. Select the corresponding ultrafiltration membrane and combine with the later drying process to prepare powdered mogroside. And other sweet ingredients.
  • the beneficial effects of the present invention are as follows: (1) Creatively realize the collection of the effective components of Luo Han Guo, and combine the aromatic volatile oil of roasted Luo Han Guo, sweet decolorization concentrated juice, pure decolorization concentrated juice, and the sweet components of mogroside in any combination.
  • the composition does not contain bitter substances, retains the flavor and nutrients of Luo Han Guo, has a strong fruit aroma and burnt aroma of Luo Han Guo, has a refreshing sweetness close to sucrose and a pure taste, the sweetness lasts for a short time, and the sweetness saturation is high.
  • Figure 1 is a gas chromatogram of Example 1 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 2 is a gas chromatogram of Example 2 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 3 is a gas chromatogram of Example 3 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 4 is a gas chromatogram of Example 4 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 5 is a high performance liquid chromatogram of Example 1 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 6 is a high performance liquid chromatogram of Example 2 of the mogroside sweetness and flavor composition of the present invention.
  • Figure 7 is a high performance liquid chromatogram of Example 3 of the mogroside sweetness and flavor composition of the present invention.
  • Fig. 8 is a high performance liquid chromatogram of Example 4 of the mogroside sweetness and flavor composition of the present invention.
  • FIG. 9 is a schematic diagram of the structure of the Luo Han Guo aromatic volatile oil collection device provided in conjunction with the Luo Han Guo curing barn according to the present invention.
  • Figure 10 is a schematic structural diagram of a Luo Han Guo aromatic volatile oil collection device provided with the Luo Han Guo oven according to the present invention.
  • the present invention is provided with the Luo Han Guo aromatic volatile oil collection device, including a stainless steel pipe 1, the first end of the stainless steel pipe 1 is connected with the exhaust hole 2 on the top of the grill 6, the end of the stainless steel pipe 1 A cooling device 3 is provided on the outer side of the pipe wall of the stainless steel pipe 1 extending out of the roasting room 6 and the stainless steel pipe 1 is provided with a stainless steel aromatic volatile oil collection for receiving a mixture of aromatic volatile oil and water at the end of the outlet
  • the storage tank 4, the side wall of the collection storage tank 4 is provided with a liquid level indicator 5 for observing the liquid level in the collection storage tank.
  • the present invention is equipped with the Luo Han Guo aromatic volatile oil collection device, and its structure is basically the same as that of the Luo Han Guo aromatic volatile oil collection device installed in the Luo Han Guo barn, except that the first end of the stainless steel pipe 1 is the same as the oven 7 vent connection.
  • the raw material used in the examples of the present invention is fresh mogroside fruit purchased from Tongdao County, Huaihua City, Hunan province, and the content of mogroside V is 0.52%.
  • the raw and auxiliary materials used in the embodiments of the present invention, unless otherwise specified, are obtained through conventional commercial channels.
  • the water vapor and the aromatic volatile oil gas generated during the roasting of Luo Han Guo enter the stainless steel pipe 1 through the exhaust hole 2 of the roasting bar 6, and the water vapor and the aromatic volatile oil gas of Luo Han Guo enter the stainless steel pipe from the head end of the stainless steel pipe 1.
  • the water vapor and the Luo Han Guo aromatic oil gas are liquefied into a liquid state, forming an oil-water mixture of water and the Luo Han Guo aromatic oil.
  • the volatile oil determination method stipulated in the Chinese Pharmacopoeia is used to determine the content of volatile oil
  • gas chromatography (GC) is used to confirm the peak position of volatile oil components
  • the content of mogroside V is determined by high performance liquid chromatography (HPLC) .
  • the gas chromatograph used was Shimadzu SHIMADZU, Japan, model: GC-2010-pro; the high performance liquid chromatograph was Agilent Technologies, model: HPLC-1260.
  • the embodiment of the mogroside sweetness and flavor composition of the present invention contains the aromatic volatile oil of mogroside, sweet flavor decolorized concentrated juice, pure decolorized concentrated juice and mogroside sweetness components, and the ratio of each component is: mogroside aromatic volatile oil 0-5 %, sweet flavor decolorizing concentrated juice 5-95%, pure flavor decolorizing concentrated juice 5-95%, mogroside sweetening ingredient 1-40%.
  • the content of mogroside V in the composition is 1-15%, and the absorbance of the diluted or dissolved aqueous solution (solid content 1% w/v) at 420 nm is less than or equal to 0.5.
  • mogroside V is 14.62% (based on the total mass of the composition).
  • the absorbance of the diluted or dissolved aqueous solution (solid content 1% w/v) at 420 nm is 0.03.
  • mogroside V is 4.95% (based on the total mass of the composition as the calculation basis; the content of mogroside V exceeds the sweet component of mogroside, because it is also contained in the aromatic volatile oil, sweet decolorization concentrated juice and pure decolorization concentrated juice of mogroside V Contains part of mogroside V).
  • the absorbance of the diluted or dissolved aqueous solution (solid content 1% w/v) at 420 nm is 0.05.
  • mogroside V is 10.51% (based on the total mass of the composition).
  • the diluted or dissolved aqueous solution (solid content 1% w/v) has an absorbance of 0.03 at 420 nm.
  • the gas chromatogram and high performance liquid chromatogram of this embodiment are shown in FIG. 3 and FIG. 7 respectively.
  • the content of mogroside V is 3.97% (based on the total mass of the composition as the calculation basis; the content of mogroside V exceeds the sweet component of mogroside, and the reason is also the same as described above, because the mogroside aromatic volatile oil, sweet flavor decolorizing concentrated juice and The pure flavor decolorizing concentrated juice also contains part of mogroside V), and the diluted or dissolved aqueous solution (solid content 1% w/v) has an absorbance of 0.02 at 420 nm.
  • the temperature is gradually increased to 47°C and maintained for 2 days to gradually evaporate the water in the Luo Han Guo and let the water vapor out;
  • the temperature is increased to 82°C and maintained for 5 hours;
  • the temperature is lowered to 73°C for 20h;
  • the temperature is lowered to 62°C, and the baking is continued for 35 hours, so that the weight of the fruit is reduced to 25% of the peeled fruit.
  • the surface is dark yellow to yellowish brown, and has a strong fruity and burnt aroma.
  • the aromatic volatile oil collecting device is used to collect the aromatic volatile oil of peeled fruit with strong fruit and burnt aroma
  • centrifugal method First use centrifugation to remove coarse particles of impurities, and then remove fine impurities through a complete set of ceramic membrane equipment, and finally obtain a clear and transparent filtrate; the centrifugal method is as follows:
  • a Decanter centrifugation filter the extract from the extraction tank through a decanter centrifuge to obtain decanter filtrate;
  • Disc centrifugation filter the decanter filtrate through disc centrifugal filtration to obtain disc filtrate;
  • cCeramic membrane clarification the dish filtrate is clarified through a complete set of ceramic membrane equipment, in which the ceramic membrane has a pore size of 0.45 ⁇ m and the material is alumina to obtain a clear and transparent ceramic membrane filtrate;
  • the ceramic membrane filtrate is cooled to 42°C, then decolorized and concentrated:
  • Ultrafiltration decolorization Decolorize the cooled ceramic membrane filtrate through a complete set of ultrafiltration membrane equipment, select the ultrafiltration membrane with a pore size of 8KD, collect the downstream liquid of the membrane, that is, the decolorization fluid, to obtain the membrane decolorization fluid;
  • Reverse osmosis membrane concentration the membrane decolorizing liquid is concentrated to 8Brix through a complete set of reverse osmosis membrane equipment to obtain 1600L membrane concentrate;
  • a Anion resin 200kg of D900 type anion resin in an anion resin column; decolorize the membrane concentrate through an anion resin. After feeding, wash the column with 600L purified water to wash out the active ingredients remaining in the column; combine the effluent and wash with water Solution to obtain anionic resin decolorizing solution;
  • b Cationic resin The cationic resin column is packed with 160kg of D717 cationic resin.
  • the anionic resin decolorizing solution is desalinated by the cationic resin.
  • the column is washed with 480L of purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain the cationic resin desalting solution;
  • a Debittering 120kg LSA-600 resin is packed in a special resin column for debittering; the cationic resin desalting solution is debittered through a special resin for debittering. After the material is fed, the column is washed with 360L purified water to wash out the effective ingredients remaining in the column. . Combine the effluent and washing liquid to obtain desalting and debittering liquid;
  • Pesticide residue removal 120kg of LSA-900 resin is packed in a special resin column for depigmentation residue removal; the debittering and desalting solution is passed through the special resin for removal of pesticide residues. After feeding, the column is washed with 360L purified water to remove the remaining residue in the column. The active ingredients are washed out; the effluent and the washing liquid are combined to obtain the desalination, debittering and de-pesticide residue liquid;
  • Activated carbon is pre-packed in the chromatography column, and then the heavy metal removal liquid is passed through the activated carbon column to remove the odor. After the material is fed, the column is washed with 24L purified water; the effluent and the washing liquid are combined and the plate and frame filter is used to obtain desalination, debittering and de-agriculture Residual heavy metal deodorant liquid;
  • the odor-removing liquid is clarified through a complete set of ceramic membrane equipment, in which the ceramic membrane has a pore size of 0.22 ⁇ m and is made of alumina to obtain a clear and transparent ceramic membrane filtrate for desalination, debittering, and removal of agricultural residues;
  • the filtrate of the desalting, debittering, agricultural residues and heavy metal removal is concentrated in vacuum, and the temperature is ⁇ 65°C, the vacuum degree is ⁇ 0.085MPa, and it is concentrated to 65Brix to obtain 130kg of sweet and decolorizing concentrated juice with desalination, bitterness, agricultural residues and heavy metals;
  • Ripe after saccharification Use the Momordica grosvenori special measuring board to classify the fresh and mature Momordica grosvenori into large, medium, small, and extrinsic fruits, and then put them in a special basket for Momordica grosvenori according to the category, and pile them in a ventilated and cool indoor place.
  • the layer is turned once every 3 days in the middle to let its water evaporate naturally and promote the conversion of internal sugar. Placed indoors for 9 days, until 50% of the fruit surface appears yellow, and water evaporation accounts for 14% of the fruit weight, that is, when the mangosteen fruit peel appears mung bean yellow, it can enter the process of extracting pure flavor decolorizing concentrated juice.
  • the ripe Luo Han Guo is crushed by a special crusher connected to the counter-current extraction tank and then enters the counter-current extraction process, according to the following operations:
  • a Decanter centrifugation filter the extraction tank extract or countercurrent extract through a decanter centrifuge to obtain decanter filtrate;
  • Disc centrifugation filter the decanter filtrate through disc centrifugal filtration to obtain disc filtrate;
  • cCeramic membrane clarification the dish filtrate is clarified through a complete set of ceramic membrane equipment, in which the ceramic membrane has a pore size of 0.45 ⁇ m and the material is alumina to obtain a clear and transparent ceramic membrane filtrate;
  • Ultrafiltration decolorization Decolorize the cooled ceramic membrane filtrate through a complete set of ultrafiltration membrane equipment, select the ultrafiltration membrane with a pore size of 10KD, and collect the downstream liquid of the membrane, that is, the decolorization fluid, to obtain the membrane decolorization fluid;
  • Reverse osmosis membrane concentration the membrane decolorizing liquid is concentrated to 10 Brix through a complete set of reverse osmosis membrane equipment to obtain 22,000L membrane concentrated liquid;
  • Anion resin The anion resin column is packed with D941 anion resin 2200kg; the membrane concentrate is decolorized by the anion resin. After feeding, the column is washed with 6600L purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain an anionic resin decolorizing liquid;
  • b Cationic resin The cationic resin column is packed with D717 cationic resin 1800kg; the anionic resin decolorizing solution is desalinated by the cationic resin. After the feed is completed, the column is washed with 5400L purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain the cationic resin desalting solution;
  • a Debittering 1600kg LSA-600 resin packed in a special resin column for debittering.
  • the cationic resin desalting solution is debittered through a special resin for debittering.
  • the column is washed with 4800L purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain a debittering, decolorizing and desalting solution;
  • De-pesticide residue 1600kg LSA-900 resin is packed with special resin column for de-pesticide residue.
  • the debittering, decolorizing and desalting solution is used to remove pesticide residues through a special resin for removing pesticide residues.
  • the column is washed with 4800L purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain the depigmented, debittered, decolorized and demineralized liquid;
  • the activated carbon is pre-packed in the chromatography column, and then the heavy metal removal liquid is passed through the activated carbon column to remove the odor. After the material is fed, the column is washed with 240L purified water; the effluent and the washing liquid are combined and filtered to obtain the removal of odor and heavy metals. Pesticide residue debittering, decolorizing and desalting liquid;
  • the ceramic membrane has a pore size of 0.22 ⁇ m and is made of alumina to obtain a clear and transparent ceramic membrane filtrate;
  • the ripe Luo Han Guo is crushed by a special crusher connected to the counter-current extraction tank and then enters the counter-current extraction process, according to the following operations:
  • a Decanter centrifugation filter the extraction tank extract or countercurrent extract through a decanter centrifuge to obtain decanter filtrate;
  • Disc centrifugation filter the decanter filtrate through disc centrifugal filtration to obtain disc filtrate;
  • the dish filtrate is clarified through a complete set of ceramic membrane equipment, in which the ceramic membrane has a pore size of 0.45 ⁇ m and is made of zirconia to obtain a clear and transparent ceramic membrane filtrate;
  • the membrane is an ultrafiltration membrane; the ceramic membrane filtrate is cooled to 40°C by passing water;
  • a High molecular weight ultrafiltration refining The cooled ceramic membrane filtrate is refined through a large molecular weight ultrafiltration membrane complete set of equipment.
  • the ultrafiltration membrane has a pore size of 8KD, and the downstream liquid of the membrane is collected to obtain the high molecular weight ultrafiltration membrane refined liquid;
  • the high molecular weight ultrafiltration membrane refined liquid is refined through a small molecular weight ultrafiltration membrane complete set of equipment, and the pore size of the ultrafiltration membrane is 2KD, and the upstream liquid of the membrane is collected to obtain 11000L small molecular weight ultrafiltration membrane refined liquid;
  • the anion resin column is packed with D941 anion resin 1000kg; the membrane concentrate is decolorized by the anion resin. After feeding, the column is washed with 3000L purified water to wash out the active ingredients remaining in the column; combine the effluent and wash with water Solution to obtain anionic resin decolorizing solution;
  • Cationic resin 850kg of cationic resin column with 001 ⁇ 16 cationic resin; Desalt the anionic resin decolorizing solution through cationic resin. After feeding, wash the column with 2500L purified water to wash out the active ingredients remaining in the column. Combine the effluent and the washing liquid to obtain a decolorizing liquid for desalination of cationic resin;
  • a Debittering 750kg of LSA-600 resin is packed in a special resin column for debittering; the decolorizing solution of cationic resin desalination is debittered through the special resin for debittering. After feeding, the column is washed with 2250L purified water to remove the remaining active ingredients in the column Wash out; Combine the effluent and the washing liquid to obtain a debittering, desalting and decolorizing solution;
  • Activated carbon is pre-packed in the chromatography column, and then the heavy metal, de-pesticide residue, debittering, desalting and decolorizing liquid is passed through the activated carbon column to remove the odor.
  • the column is washed with 300L purified water; the effluent and washing liquid are combined, and the plate and frame filter , It is necessary to remove the peculiar smell, heavy metals, pesticide residues, bitterness, desalting and decolorization liquid
  • the membrane is a nanofiltration membrane
  • the vacuum concentrate is spray-dried to obtain the finished product-mogroside sweetness ingredient, the product weight is 165kg;
  • (V) Mogroside sweetness and flavor composition mixing the mogroside aromatic volatile oil obtained in step I, the sweet decolorizing concentrated juice obtained in step II, the pure decolorizing concentrated juice obtained in step III, and the mogroside sweetening components obtained in step IV are combined according to Mouthfeel, smell, sweetness persistence, and product existence form requirements are mixed to obtain mogroside sweetness and flavor composition.
  • Example 1 Example 2, Example 3, and Example 4 in the first part of the mogroside sweetness and flavor composition examples of the present invention.

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Abstract

罗汉果苷甜味和风味组合物及其制备方法与应用。所述组合物包括有罗汉果芳香挥发油、罗汉果甜香脱色浓缩汁、罗汉果纯味脱色浓缩汁、罗汉果苷甜味成分中的至少一种,其中罗汉果甜香脱色浓缩汁、罗汉果纯味脱色浓缩汁和罗汉果苷甜味成分≠0。该组合物不含苦味物质,保留了罗汉果的风味和营养成分,具有浓郁的果香味和焦香味,具有接近蔗糖的清爽甜味和纯正口感,甜味持续时间短,甜味饱和度高,集罗汉果的香、甜、味、营养于一体;制备工艺简单,成本较低。罗汉果苷甜味和风味组合物可广泛应用于食品、饮品、乳品、保健品和药品等领域。

Description

罗汉果苷甜味和风味组合物及其制备方法与应用 技术领域
本发明涉及一种罗汉果苷甜味和风味组合物及其制备方法,以及该组合物的应用,尤其是涉及一种由罗汉果芳香挥发油、甜香脱色浓缩汁、纯味脱色浓缩汁及罗汉果苷甜味成分组配而成的罗汉果苷甜味和风味组合物,及以鲜罗汉果或无籽罗汉果为原料提取罗汉果芳香挥发油、甜香脱色浓缩汁、纯味脱色浓缩汁和罗汉果苷甜味成分的方法,以及所述罗汉果苷甜味和风味组合物在食品、饮品、乳品、保健品和药品中的应用。
背景技术
罗汉果(Siraitia grosvenorii(Swingle)C.Jeffrey),英文名:fructus momordicae,葫芦科多年生藤本植物的果实。别名拉汗果、假苦瓜、光果木鳖、金不换、罗汉表、裸龟巴,被人们誉为“神仙果”,其叶心形,雌雄异株,夏季开花,秋天结果。主要产于广西壮族自治区桂林市永福县龙江乡、百寿镇,龙胜各族自治县,以及湖南省怀化、永州、邵阳等地。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。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。
无籽罗汉果,系将罗汉果的三倍体植株和二倍体雄株进行种植,开花时用二倍体的雄株对三倍体的雌株人工授粉,雌株挂果后得到无籽罗汉果。
罗汉果及无籽罗汉果含有丰富的风味和营养成分,以及三萜皂苷类非糖甜味成分。
一、挥发油成分
罗汉果果实含挥发油0.2%~0.3%,挥发油成分达20余个,从中鉴定出13个主要成分:十一醇、库贝醇、丁基酚酮、T-紫穗槐醇、1-萘酚、1,2,3,4,4a,7,8,8a,-八氢-1,6二甲基-4-(1-甲基乙基)-雪松醇、环丙甲酸十三烷酯、十五烷酸、n-三十七烷醇、十六烷酸甲酯、n-十六烷酸、9,12-十八碳二烯酸甲酯、9,12-十八碳二烯酸,共占挥发油总量的94.96%。其中,:n-十六烷酸(45.609%)和9,12-十八碳二烯酸(36.151%)是主要成分,它们共占挥发油总量的81.76%。
无籽罗汉果的挥发油组成与罗汉果相似,但是含量有所变化,目前已鉴定其中的24个成分。其中包括:乙二醇异丙醚(27.21%)、1,2-苯二甲酸丁基-2-乙基己酯(13.51%)、邻苯二甲酸二异丁酯(10.85%)、天竺葵醛(10.22%),(E)3-葵烯酸(6.52%)、丁酸丁酯(4.99%)、乙酸-2-十三烷酯(4.86%),它们共占挥发油总量的78.16%。
二、化学成分
罗汉果及无籽罗汉果均含有罗汉果三萜皂苷,还有葡萄糖(glucose),果糖(fructose) 占14%,十多种人体必需氨基酸、蛋白质、脂肪酸、黄酮类化合物、维生素C以及锰、铁、镍、硒、锡、碘、钼等26种无机元素和微量元素等。
葫芦素烷三萜类:这类化合物是罗汉果中主要有效成分,它们有共同的苷元结构。罗汉果中这类物质除少数外,均为甜味物质或微甜物质。其中罗汉果苷V是主要的甜味成分,它无毒、低热量、高甜度、热稳定性好,是一种天然甜味剂物质。
蛋白质、氨基酸:罗汉果干果中含蛋白质7.1%-7.8%。在其水解物中,除色氨酸未被测定外,18种氨基酸齐全。在测定的氨基酸中,含量较高的有谷氨酸(108.2-113.3mg/kg)、天冬氨酸(93.9-112.5mg/kg)、缬氨酸(52.5-55.5mg/kg)、丙氨酸(49.9-66.8mg/kg)、亮氨酸(48.5-56.7mg/kg)。谷氨酸是人体中需要量最大的非必需氨基酸,是合成谷胱甘肽的重要原料,可见,罗汉果具有较高的营养价值。
无机元素:罗汉果果实中含有24种无机元素,其中人体必需的微量元素和广泛元素有16种,含量较高的元素有钾(12290mg/kg)、钙(667mg/kg)、镁(550mg/kg)。罗汉果中含有的硒达到0.186mg/kg,是粮食的2倍-4倍,而元素硒在冠心病防治、抗衰老、抗癌方面有较好的疗效。
三、罗汉果苷等非糖甜味成分
罗汉果果实中含非糖甜味成分,主要是三萜皂苷类:罗汉果苷(mogroside)V及IV。罗汉果苷V的甜度是蔗糖(srcrose)的256-344倍,罗汉果苷IV的甜度为蔗糖的126倍;次要的是D-甘露醇(D-mannitol),其甜度为蔗糖的0.55-0.65倍。
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)。
中文名称:罗汉果苷V
英文名称:Mogroside V
CAS No.:88901-36-4
分子式:C 60H 102O 29
Figure PCTCN2019111855-appb-000001
目前国内外对罗汉果和无籽罗汉果研究很多,市场上也有多种规格的罗汉果提取物销售。但研究的重点是罗汉果皂苷的分离提纯以及罗汉果浓缩汁,且市场上销售的罗汉果提取物主要是普通规格的罗汉果浓缩汁以及罗汉果苷V20%~60%含量的粉末状规格。
CN201810969469、CN201810320300、CN201710743703、CN201710469860、CN201710277285、CN201210207266、CN200810097509等公开的技术方案,均是以提取罗汉果浓缩汁为方向。这类技术所生产的罗汉果浓缩汁,由于没有收集罗汉果芳香挥发油,且罗汉果芳香挥发油在生产过程中大量损失,在前处理工艺中也未有将罗汉果增香增味的去皮干燥工艺,导致最终产品罗汉果浓缩汁既无烘焙罗汉果的芳香味,也无去皮干燥罗汉果的焦香味,以致于风味欠缺,口感稍差。
CN201811397385、CN201811250821、CN201711214793、CN201710388435、CN201610387839、CN02128065等公开的技术方案,均是以提纯罗汉果苷V为方向。这类技术所生产出来的罗汉果提取物,是以提取罗汉果皂苷类甜味成分为主,完全去除了罗汉果的风味和营养成分,仅仅是作为甜味剂使用的。且由于甜味成分较纯,导致甜味持续时间长,非所有人群能接受,不是风味和营养型的罗汉果提取物。
发明内容
本发明所要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种罗汉果苷甜味和风味组合物,该组合物不含苦味物质,但保留了罗汉果的特有风味和营养成分,具有浓郁的罗汉果的特有果香味和焦香味,具有接近蔗糖的清爽甜味和纯正口感,甜味持续时间较短,集罗汉果的香、甜、味、营养成分于一体。
本发明进一步要解决的技术问题是,提供一种罗汉果罗汉果芳香挥发油、甜香脱色浓缩汁、纯味脱色浓缩汁、罗汉果苷甜味成分的制备方法。
本发明解决其技术问题所采用的技术方案是:一种罗汉果苷甜味和风味组合物,包括罗汉果芳香挥发油、甜香脱色浓缩汁、纯味脱色浓缩汁、罗汉果苷甜味成分中的至少一种,其中甜香脱色浓缩汁、纯味脱色浓缩汁和罗汉果苷甜味成分≠0。
进一步,所述组合物中,以罗汉果苷甜味和风味组合物的总质量为计算基准,罗汉果苷V的质量含量为1%~15%。
进一步,所述组合物中,含有罗汉果挥发油成分n-十六烷酸或/和9,12-十八碳二烯酸,或无籽罗汉果挥发油成分乙二醇异丙醚、1,2-苯二甲酸丁基-2-乙基己酯、邻苯二甲酸二异丁酯、天竺葵醛中的一种,或所述罗汉果挥发油几种成分的组合,所述挥发油的总质量含量为0%~5%;优选0.5%~4.0%。
本发明进一步解决其技术问题采用的技术方案是,一种罗汉果苷甜味和风味组合物的制备方法,包括以下步骤:(I)罗汉果芳香挥发油收集;(II)罗汉果甜香脱色浓缩汁的提取精制;(III)罗汉果纯味脱色浓缩汁的提取精制;(IV)罗汉果苷甜味成分的提取精制;(V)混配。
进一步,步骤(I)中,所述罗汉果芳香挥发油收集的方法是:
(1)糖化后熟:将鲜罗汉果用筐装好,层堆在室内通风阴凉处,让罗汉果中的水分自然蒸发,促进内部糖分的转化,至罗汉果果皮呈现绿豆黄色;
优选方案:用罗汉果专用量果板对鲜罗汉果按大、中、小、外果进行分类;然后按类分别用罗汉果专用筐装好;层堆的层数为2~4层,在室内放置天数为7~10天,中间每隔3~4天翻动一次;至果实表面有≥50%面积呈现黄色,水分蒸发失重占果重的10~15%;
进一步的优选方案:用罗汉果专用量果板对对鲜罗汉果按大、中、小、外果进行分类,以提高分类效率;
(2)烤房烘烤与芳香挥发油收集:将经步骤(1)糖化后熟的罗汉果果实,按照大、中、小、外果类别,分别装入网盘,然后置于设有芳香挥发油收集装置的烤房的网盘放置架上,点火升温烘烤;
在罗汉果烘烤过程中,罗汉果所含芳香挥发油会随同逐步挥发、蒸发,经冷却,形成芳香挥发油和水的混合物,通过烤房所设芳香挥发油收集装置予以收集,得罗汉果芳香挥发油;烘烤完毕,还得罗汉果干果;
烘烤方法优选方案:在烘烤过程中,烘烤的升温降温过程,分为以下三个阶段:
第一阶段:升温至45℃~50℃维持2~3天,使罗汉果中的水分和芳香挥发油开始逐步排出、蒸发、挥发;
第二阶段:逐步提高温度至65℃~70℃,持续2~3天,使水分和芳香挥发油加快排出、蒸发、挥发;
第三阶段:降温至55℃~60℃,继续烘烤,使果实的重量下降到相当鲜果的25~30%,然后停火,自然降温至环境温度,出炉;
所述芳香挥发油收集装置优选方案:采用以下构件构成:包括不锈钢导管,所述不锈钢导管的首端与烤房顶部的排气孔连接,不锈钢导管的尾端伸出烤房之外,伸出烤房之外的不锈钢导管的管壁外侧设有冷却装置,不锈钢导管的尾端出口处设有接收芳香挥发油与水混合物的芳香挥发油收集储罐,所述芳香挥发油收集储罐侧壁设有用于观察收集储罐内液位的液位指示器。
进一步,步骤(II)中,所述甜香脱色浓缩汁的提取精制方法包括以下步骤:糖化后熟;专用烤箱去皮烘烤;提取;离心过滤与陶瓷膜澄清;膜分离与浓缩;树脂脱色;树脂脱苦、脱农残、脱重金属;活性炭去异味;陶瓷膜澄清;真空浓缩;
优选方案:
(1)糖化后熟:操作方法同步骤(I)的(1)糖化后熟;
(2)烤箱烘烤与芳香挥发油收集:将糖化后熟的罗汉果果实,剥去果皮,铺摊成片状或块状,再分别装入网盘,用烤箱烘烤,得去皮罗汉果干果;
在烘烤过程中,去皮罗汉果所含芳香挥发油会随同水分逐步同时挥发、蒸发,经冷却,形成芳香挥发油和水的混合物,通过所设芳香挥发油收集装置予以收集,得罗汉果芳香挥发油;
铺摊优选方案:按照大、中、小、外果分类,进行铺摊;
烘烤方法优选方案:在烘烤过程中,烘烤的升温降温过程,分为以下三个阶段:
第一阶段:升温到80℃~85℃,维持4~8h;
第二阶段:降温到75℃~70℃,持续16~24h;
第三阶段:降温到65℃~60℃,继续烘烤30~40h,使果实的重量下降到相当去皮果重量的20~30%,表面呈深黄色至黄褐色,并具有浓郁的果香味和焦香味时,停止烘烤,自然降温,出箱;
芳香挥发油收集装置结构优选方案:采用以下构件构成:包括不锈钢导管,所述不锈钢导管的首端与烤箱顶部的排气孔连接,不锈钢导管的尾端伸出烤房之外,伸出烤房之外的不锈钢导管的管壁外侧设有冷却装置,不锈钢导管的尾端出口处设有接收芳香挥发油和水混合物的芳香挥发油收集储罐;所述芳香挥发油收集储罐侧壁设有用于观察收集储罐内液位的液位指示器;
(3)甜香脱色浓缩汁的提取、精制:
A.提取
采用提取罐提取或逆流提取槽提取:
a)提取罐提取:将步骤(II)的步骤(2)所得去皮罗汉果干果投入提取罐中,加水 搅拌,再进行固液分离,得提取罐提取液;
优选方案:所述水为纯化水;提取温度优选80℃~95℃;提取次数3次,每次提取时间分别为1.5~2.5h、1.0~2.0h、0.5~1.5h;每次纯化水加入体积量分别为去皮罗汉果干果重量的8~10倍、7~9倍、5~7倍;每次提取完成后,过滤,滤渣进入下一次提取,第三次提取完成后,滤渣另行处理;合并3次提取液,即得提取罐提取液;
b)逆流提取槽提取:将步骤(II)的步骤(2)所得去皮罗汉果干果投入逆流提取槽中,加水进行逆流提取;
优选方案:所述水为纯化水;提取温度优选80℃~95℃;提取时间1.5-2.5h;纯化水加入体积量为去皮罗汉果干果重量的4~6倍(纯化水体积/干燥的去皮果,V/W);提取完成后,过滤,滤渣另行处理;合并不断流出的提取液,得逆流提取槽提取液;
B.离心过滤与陶瓷膜澄清
先离心,去除提取罐提取液或逆流提取液中的杂质,再通过陶瓷膜成套设备去除其中的细微杂质,最终得到澄清透明的滤液;
优选方案:
a)卧螺离心:将提取罐提取液或逆流提取液通过卧螺离心机过滤,得卧螺离心滤液;
b)碟式离心:将卧螺滤液通过碟式离心过滤,得碟式离心滤液;
c)陶瓷膜澄清:将碟式滤液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.45μm,材质为氧化铝或氧化锆,得澄清透明的陶瓷膜滤液;
C.膜分离与浓缩
将陶瓷膜滤液通过水冷却,再用超滤膜通过膜分离去除大部分色素,然后用反渗透膜浓缩,方便脱色及后续操作;
优选方案:
a)将陶瓷膜滤液通过水冷却至45℃以下;
b)超滤脱色:将冷却好的陶瓷膜滤液通过超滤膜成套设备脱色,选择超滤膜孔径8KD~10KD,收集膜下游液即脱色液,得膜脱色液;
c)反渗透膜浓缩:将膜脱色液通过反渗透膜成套设备浓缩至5~10Brix,得膜浓缩液;
D.树脂脱色
通过阴离子树脂和阳离子树脂脱色,以得到接近无色的脱色液;
优选方案:所述阴离子树脂包括凝胶型及大孔型丙烯酸弱碱阴离子树脂、丙烯酸系强碱和弱碱阴离子树脂、凝胶型及大孔型苯乙烯系强碱阴离子树脂、大孔型丙烯酸强碱阴离子树脂、大孔型苯乙烯系弱碱阴离子树脂;
所述阳离子树脂包括凝胶型及大孔型苯乙烯系强酸阳离子树脂、丙烯酸系凝胶型和大孔型弱酸阳离子树脂;
阴离子树脂优选型号:D900、D941、D316、D296;
阳离子树脂优选型号:001×16,D717;
进一步的优选方案:
a)阴离子树脂用量为:每1000kg去皮罗汉果干果用350kg~5500kg;将膜浓缩液通过阴离子树脂脱色,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阴离子树脂脱色液;
b)阳离子树脂用量为:每1000kg去皮罗汉果干果用250kg~450kg;将阴离子树脂脱色液通过阳离子树脂脱盐,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阳离子树脂脱盐液;
E.树脂脱苦、脱农残、脱重金属
通过树脂进一步脱苦、脱农残、脱重金属,使之口感良好,农残、重金属含量达标;
优选方案:所述脱苦、脱农残、脱重金属所用树脂包括凝胶型及大孔型丙烯酸树脂、丙烯酸系树脂、凝胶型及大孔型苯乙烯系树脂、大孔型丙烯酸树脂、大孔型苯乙烯系树脂、丙烯酸系凝胶型树脂;
脱苦专用树脂优选型号:LSA-600、LX-900;
脱农残专用树脂优选型号:LSA-900B、LSA-900D;
脱重金属专用树脂优选型号:LX-500、LSC-As、LSC-400;
进一步的优选方案:
a)使用脱苦专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将阳离子树脂脱盐液通过脱苦专用树脂柱脱苦,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得脱苦液;
b)使用脱农残专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将脱苦液通过脱农残专用树脂柱脱农残,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱苦脱农残液;
c)使用脱重金属专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将脱苦脱农残液通过脱重金属专用树脂柱脱重金属,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱苦脱农残脱重金属液;
F.活性炭去异味
活性炭用量为,每1000kg去皮罗汉果干果用活性炭12kg~20kg;所述活性炭为粒状活 性炭;
优选方案:预先将活性炭装于层析柱内,然后将脱苦脱农残脱重金属液通过活性炭柱去异味,进完料以后,再用纯化水洗柱;合并流出液和水洗液,板框过滤,得脱苦脱农残脱重金属去异味液;
G.陶瓷膜澄清
将脱苦脱农残脱重金属去异味液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.22μm,材质为氧化铝或氧化锆,得澄清透明的陶瓷膜滤液;
H.真空浓缩
将陶瓷膜滤液真空浓缩,控制温度≤65℃,真空度≥0.085MPa,浓缩至60~70Brix,即得甜香脱色浓缩汁。
进一步,步骤(III)中,所述纯味脱色浓缩汁提取精制的方法包括以下步骤:以新鲜成熟的罗汉果为原料,糖化后熟;再用提取罐提取或逆流提取槽提取;离心过滤与陶瓷膜澄清;膜分离与浓缩;树脂脱色;树脂脱苦、脱农残、脱重金属;活性炭去异味;陶瓷膜澄清;真空浓缩;
优选方案:
(1)糖化后熟:同步骤(I)的(1)糖化后熟;
(2)提取
将糖化后熟的罗汉果通过破碎机破碎后进入提取工序;
优选方案:
a)提取罐提取:操作方法基本同步骤(II)的(3)甜香脱色浓缩汁A.提取项下a)提取罐提取,所不同的是,此处原料是鲜罗汉果,且纯化水加入体积量分别为罗汉果质量的2~4倍、2~4倍、2~3倍;
b)逆流提取槽提取:操作方法基本同步骤(II)的(3)甜香脱色浓缩汁A.提取项下b)逆流提取槽提取,所不同的是纯化水加入体积量为鲜罗汉果质量的1.2~2.0倍;
(3)离心过滤与陶瓷膜澄清
同步骤(II)的(3)甜香脱色浓缩汁B.离心过滤与陶瓷膜澄清;
(4)膜分离与浓缩
同步骤(II)的(3)甜香脱色浓缩汁C.膜分离与浓缩;
(5)树脂脱色
操作方法基本同步骤(II)的(3)甜香脱色浓缩汁D.树脂脱色,所不同的是,更优选的方案:
a)阴离子树脂:阴离子树脂用量为每1000kg鲜罗汉果用阴离子树脂90kg~150kg;
b)阳离子树脂:阳离子树脂用量为每1000kg鲜罗汉用60kg~120kg;
(6)树脂脱苦、脱农残、脱重金属
操作方法基本同步骤(II)的(3)甜香脱色浓缩汁E.树脂脱苦、脱农残、脱重金属,所不同的是,更优选的方案:
a)脱苦:树脂用量为每1000kg鲜罗汉果用树脂60kg~90kg;
b)脱农残:树脂用量为每1000kg鲜罗汉果用树脂60kg~90kg;
c)脱重金属:树脂用量为每1000kg鲜罗汉果用树脂60kg~90kg;
(7)活性炭去异味
操作方法基本同步骤(II)的(3)甜香脱色浓缩汁F.活性炭去异味,所不同的是活性炭用量为,每1000kg鲜罗汉果用活性炭3~5kg;
(8)陶瓷膜澄清
同步骤(II)的(3)甜香脱色浓缩汁G.陶瓷膜澄清;
(9)真空浓缩
同步骤(II)的(3)甜香脱色浓缩汁H.真空浓缩。
进一步,步骤(IV)中,所述罗汉果苷甜味成分的提取精制方法,包括以下步骤,将新鲜成熟的罗汉果糖化后熟,提取罐或逆流提取槽提取,离心过滤与陶瓷膜澄清,膜分离精制,树脂脱色,树脂脱苦、脱农残、脱重金属,活性炭去农残及脱异味,陶瓷膜澄清,膜分离脱杂味,真空浓缩,干燥;
优选方案:
(1)糖化后熟:同步骤(I)的(1)糖化后熟;
(2)提取
采用以下两种方法中的一种:
a)提取罐提取:操作方法同步骤(III)的(2)提取a)提取罐提取;
b)逆流提取槽提取:操作方法同步骤(III)的(2)提取b)逆流提取槽提取;
(3)离心过滤与陶瓷膜澄清
操作方法同步骤(III)的(3)离心过滤与陶瓷膜澄清;
(4)膜分离精制
所述膜为超滤膜;将陶瓷膜滤液通水冷却,根据罗汉果苷甜味成分分子分量大小差异,先用大分子量的超滤膜进行分子截留,去除大部分色素和杂质,再用小分子量的超滤膜进行分子截留,收集罗汉果苷甜味成分;
优选方案:
a)大分子量超滤精制:将冷却至45℃以下的陶瓷膜滤液,通过大分子量超滤膜成套设备精制,选择超滤膜孔径8KD~10KD,收集膜下游液即精制液,得大分子量超滤膜精制液;
b)小分子量超滤精制及浓缩:将大分子量超滤膜精制液通过小分子量超滤膜成套设备精制,选择超滤膜孔径2KD~3KD,收集膜上游液即精制液,得小分子量超滤膜精制液;
(5)树脂脱色
操作方法同步骤(III)的(5)树脂脱色;
(6)树脂脱苦、脱农残、脱重金属
操作方法同步骤(III)的(6)树脂脱苦、脱农残、脱重金属;
(7)活性炭去农残及脱异味
操作方法同步骤(III)的(7)活性炭去异味;
(8)陶瓷膜澄清
操作方法同步骤(III)的(8)陶瓷膜澄清;
(9)膜分离脱杂味
优选方案:
所述膜为纳滤膜;
将陶瓷膜滤液通过纳滤膜成套设备,浓缩至原体积1/4,去除小分子物质和杂味;
(10)真空浓缩
优选方案:
将膜分离液真空浓缩,控制温度≤65℃,真空度≥0.085MPa,浓缩至17~25波美,得真空浓缩液;
(11)干燥
将真空浓缩液喷雾干燥或微波真空干燥,得罗汉果苷甜味成分产品。
进一步,步骤(V),所述混配是指,将收集的烘焙罗汉果的芳香挥发油、提取精制的甜香脱色浓缩汁、纯味脱色浓缩汁、罗汉果苷甜味成分,根据所需产品口感、气味、甜度持久性、产品存在形式要求,确定各组分具体配比,进行混配。
本发明罗汉果苷甜味和风味组合物可广泛应用于食品、饮品、乳品、保健品和药品等领域。
本发明制备方法的步骤(I)中,关于罗汉果烘焙,芳香挥发油的收集,本发明者的研究表明,罗汉果烘焙过程中,会散发出来具有浓郁果香味和焦香味的罗汉果芳香挥发油气 味;现有罗汉果浓缩汁或粉末状罗汉果提取物均无此特异罗汉果果香味和焦香味,于是,本发明者设计了专用装置用于收集烘焙过程中的芳香挥发油,并将此挥发油添加于罗汉果提取物中,以增强罗汉果提取物的特有香气,改善口感,对罗汉果相关产品的品质进行提升。
步骤(II)中,关于甜香脱色浓缩汁的提取精制,本发明者的研究表明,去皮干燥的罗汉果,即表面呈现棕黄色至棕褐色的去皮罗汉果,在泡茶后,具有特别清爽的甜味,并还原了罗汉果的特殊果香味和焦香味。于是,本发明者改变以往直接以鲜罗汉果提取罗汉果浓缩汁的工艺,先将鲜罗汉果去皮烘烤,使鲜罗汉果具有特殊的甜香味和焦香味,以及纯正的甜味口感,之后再用专有的提取分离工艺生产出具有甜香味的脱色浓缩汁。
同时,本发明者的研究还表明,发现去皮罗汉果在烘烤过程中,也有罗汉果所特有的果香味和焦香味产生,于是,将去皮罗汉果在烘烤过程中所产生的挥发油也予以收集,以尽可能得到罗汉果的全部有效活性成分。
步骤(II)中,虽然此处原料为干燥的去皮罗汉果,区别以鲜罗汉果为原料破碎提取,但因在前期干燥过程中已去皮,且经实验证明,所述提取方法可以完全将去皮干燥的罗汉果成分完全提取出来。
步骤(II)~(IV)中,所述离心过滤与陶瓷膜澄清,优选先用卧螺离心过滤,再用碟式离心过滤,最后再进入陶瓷膜澄清,使用上有相应顺序,效果最佳。
步骤(II)~(IV)中,所述陶瓷膜澄清均2次用到,但是,优选的陶瓷膜孔径不同,第1次是0.45μm,第2次是0.22μm,目的是为了完全除尽生产过程中所产生的微细颗粒沉淀,以得到完全澄清透明的产品。
步骤(II)~(III)中,所述膜分离与浓缩,优选先采用孔径为8KD~10KD的超滤膜,分离去除色素以及大分子杂质,再通过反渗透膜浓缩,得到相应浓度的膜浓缩液。
步骤(IV)中,所述膜分离精制,优选先采用8KD~10KD的超滤膜,分离去除色素以及大分子杂质,收集的是膜下游液体,即透过液;然后再过2KD~3KD的超滤膜,分离去除葡萄糖、果糖,氨基酸等成分,收集的是膜上游液体,即截留液。因罗汉果苷等甜味成分的平均分子量约1200,加上分子结构特点,选择此范围的超滤膜能得到纯化的罗汉果苷等甜味成分而去除其余大部分杂质。
步骤(II)~(IV)中,所述活性炭为粒状活性炭,而非粉末活性炭。所用粒状活性炭的目的是改善味道以及去除极少量的农残,不是用来脱色。
步骤(IV)中,所述干燥方式为喷雾干燥或微波真空干燥,其余干燥方式效果欠佳。
本发明组合物中,罗汉果苷V含量优选为1%~15%(w/w),稀释或溶解的水溶液,固 体含量1%w/v在420nm处的吸光度≤0.5。其中所述罗汉果苷V含量根据《中国药典》标准用HPLC法测定。
本发明组合物中含有或不含n-十六烷酸、9,12-十八碳二烯酸等罗汉果挥发油成分或乙二醇异丙醚、1,2-苯二甲酸丁基-2-乙基己酯、邻苯二甲酸二异丁酯、天竺葵醛等无籽罗汉果挥发油成分以及罗汉果和无籽罗汉果挥发油成分的组合,总挥发油含量为0%~5%,其中所述挥发油含量根据《中国药典》标准用挥发油测定法测定,单一组分挥发油含量用GC法测定。
本发明的原理:
本发明以罗汉果或/和无籽罗汉果为原料。研究表明,罗汉果和无籽罗汉果含有多种挥发油,具有特殊的芳香气味,但在鲜果中无法体现出芳香味和焦香味,只有在烘烤过程中及烘烤后,人们才能闻到其明显的芳香味和焦香味。由此,我们可以在基本不增加成本的情况下,在对罗汉果、无籽罗汉果进行烘烤的过程中,收集烘焙果和去皮果的芳香挥发油,然后作为原料添加到本发明组合物中,或作其它用途。
研究表明,罗汉果经去皮烘焙以后,具有特殊的甜香味,而此味道在本发明工艺条件下,能很好地保留下来,使用本发明烘焙前处理工艺及提取精制方法,可以得到具有甜香味的脱色浓缩汁。
罗汉果中含有的营养成分和罗汉果苷等甜味成分易溶于水中,可以通过水提取出来。水提液中含有浑浊物质,必须进行精制。例如,经过二级离心和陶瓷膜澄清,才能得到澄清透明的液体,否则易堵塞陶瓷膜设备。通过超滤膜的分子量截留技术,可以将大部分色素和大分子杂质去除,而易于后期的树脂脱色。为了减少进层析柱的液体体积和使色素集中以提高脱色效果,可以用反渗透膜浓缩前述膜脱色液。研究表明,阴离子树脂对经膜分离脱色后的罗汉果脱色液具有脱色作用,而优选特定型号的阴离子树脂,脱色效果更佳。通过阴离子树脂交换吸附,色素被树脂吸附,而罗汉果苷等甜味物质以及营养物质不被吸附而流出,再利用阳离子树脂将经阴离子树脂处理的脱色液pH值恢复到初始状态,即实现了体系的酸碱还原。罗汉果原生状态会存在极少量的苦味成分,以及农残,重金属,这些有害物质会一直存在于工艺过程中,因此,要将这些物质去除,以使产品中的这些物质含量达标。在这些步骤之后,通过粒状活性炭进一步改善产品的味道,或同时去除残存的农残,以得到接近完美的甜香脱色浓缩汁和纯味脱色浓缩汁。
而提取的罗汉果苷等甜味成分以粉末形式存在,工艺上与所述甜香脱色浓缩汁和纯味脱色浓缩汁有区别。如果将所述甜香脱色浓缩汁和纯味脱色浓缩汁直接进行干燥,则无法达到预期的干燥目的,因其中含有大量低碳糖等成分,因此,需要将这些物质去除。而适 当规格的超滤膜可以保留平均分子量1200左右的罗汉果苷等甜味成分,而让低碳糖等物质去除,选择相应的超滤膜,结合后期的干燥工艺,可以制备粉末状的罗汉果苷等甜味成分。
本发明的有益效果如下:(1)创造性地实现了罗汉果各有效成分的集合,将烘焙罗汉果的芳香挥发油、甜香脱色浓缩汁、纯味脱色浓缩汁、罗汉果苷甜味成分,任意组合,该组合物不含苦味物质,保留了罗汉果的风味和营养成分,具有浓郁的罗汉果果香味和焦香味,具有接近蔗糖的清爽甜味和纯正口感,甜味持续时间较短,甜味饱和度高,集罗汉果的香、甜、味、营养于一体,优于现有罗汉果浓缩汁和罗汉果提取物,市场前景看好;(2)生产工艺简单,易于操作和实现;且生产成本低,适合工业化生产;所得组合物中,罗汉果苷V优选含量为1%~15%(w/w),稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度≤0.5;产品收率以罗汉果苷V计,≥85%;(3)本发明,仅使用水这1种溶剂,因不使用普通大孔吸附树脂,故不使用乙醇,最大限度地保留了罗汉果浓缩汁和罗汉果苷甜味成分的天然属性;(4)生产成本低,提高了企业的经济和社会效益。
附图说明
图1为本发明罗汉果苷甜味和风味组合物实施例1的气相色谱图;
图2为本发明罗汉果苷甜味和风味组合物实施例2的气相色谱图;
图3为本发明罗汉果苷甜味和风味组合物实施例3的气相色谱图;
图4为本发明罗汉果苷甜味和风味组合物实施例4的气相色谱图;
图5为本发明罗汉果苷甜味和风味组合物实施例1的高效液相色谱图;
图6为本发明罗汉果苷甜味和风味组合物实施例2的高效液相色谱图;
图7为本发明罗汉果苷甜味和风味组合物实施例3的高效液相色谱图;
图8为本发明罗汉果苷甜味和风味组合物实施例4的高效液相色谱图;
图9为本发明与罗汉果烤房配套设置的罗汉果芳香挥发油收集装置的结构示意图;
图10为本发明与罗汉果烤箱配套设置的罗汉果芳香挥发油收集装置的结构示意图。
具体实施方式
下面结合附图和实施例对本发明作进一步详细说明。
参照图9,本发明与罗汉果烤房配套设置的罗汉果芳香挥发油收集装置,包括不锈钢导管1,所述不锈钢导管1的首端与烤房6顶部的排气孔2连接,不锈钢导管1的尾端伸出烤房6之外,伸出烤房6之外的不锈钢导管1的管壁外侧设有冷却装置3,不锈钢导管1的尾端出口处设有接收芳香挥发油与水混合物的不锈钢芳香挥发油收集储罐4,所述收集储罐4的侧壁设有用于观察收集储罐内液位的液位指示器5。
参照图10,本发明与罗汉果烤箱配套设置的罗汉果芳香挥发油收集装置,其结构与罗汉果烤房配套设置的罗汉果芳香挥发油收集装置的结构基本相同,区别仅在于,不锈钢导管1的首端是与烤箱7的排气孔连接。
本发明实施例所使用的原料鲜罗汉果购于湖南省怀化市通道县,其中罗汉果苷V的含量为0.52%。本发明实施例所使用的原辅材料,如无特殊说明,均通过常规商业途径获得。
工作时,罗汉果烘烤过程中产生的水蒸气和罗汉果芳香挥发油气体通过烤房6的排气孔2进入不锈钢导管1,水蒸气和罗汉果芳香挥发油气体进入不锈钢导管后,从不锈钢导管1的首端沿不锈钢导管1的中段向尾端方向流动,靠近不锈钢导管1的尾端时,在冷却装置3的冷却下,水蒸气和罗汉果芳香挥发油气体液化为液态,形成水和罗汉果芳香挥发油的油水混合物,落入不锈钢芳香挥发油收集储罐4中;通过设于芳香挥发油收集储罐4侧壁的液位指示器5,可以观察到芳香挥发油收集储罐4所收集的所述油水混合物的数量。
本发明实施例中,采用《中国药典》规定的挥发油测定法测定挥发油含量,用气相色谱法(GC)进行挥发油成分的峰位确认,用高效液相色谱法(HPLC)测定罗汉果苷V的含量。所用气相色谱仪为日本岛津SHIMADZU,型号:GC-2010-pro;高效液相色谱仪为安捷伦科技有限公司Agilent technologies,型号:HPLC-1260。
一、本发明罗汉果苷甜味和风味组合物的实施例:
本发明罗汉果苷甜味和风味组合物实施例,含罗汉果芳香挥发油,甜香脱色浓缩汁、纯味脱色浓缩汁和罗汉果苷甜味成分,所述各组分配比为:罗汉果芳香挥发油0~5%,甜香脱色浓缩汁5~95%、纯味脱色浓缩汁5~95%、罗汉果苷甜味成分1~40%。该组合物中罗汉果苷V含量1~15%,稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度≤0.5。
以下为罗汉果苷甜味和风味组合物4个具体实施例的质量百分比配比:
实施例1
罗汉果芳香挥发油1%,甜香脱色浓缩汁30%、纯味脱色浓缩汁40%、罗汉果苷甜味成分29%。其中罗汉果苷V含量14.62%(以该组合物总质量为计算基准)。稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度为0.03。
本实施例的气相色谱图和高效液相色谱图分别如图1和图5所示。
实施例2
罗汉果芳香挥发油2%,甜香脱色浓缩汁50%、纯味脱色浓缩汁45%、罗汉果苷甜味成分3%。其中罗汉果苷V含量4.95%(以该组合物总质量为计算基准;罗汉果苷V含量超过所述罗汉果苷甜味成分,是因为罗汉果芳香挥发油、甜香脱色浓缩汁和纯味脱色浓缩 汁中也含有部分罗汉果苷V)。稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度0.05。
本实施例的气相色谱图和高效液相色谱图分别如图2和图6所示。
实施例3
罗汉果芳香挥发油3%,甜香脱色浓缩汁60%、纯味脱色浓缩汁20%、罗汉果苷甜味成分17%。其中罗汉果苷V含量10.51%(以该组合物总质量为计算基准)。稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度0.03。
本实施例的气相色谱图和高效液相色谱图分别如图3和图7所示。
实施例4
罗汉果芳香挥发油4%,甜香脱色浓缩汁85%、纯味脱色浓缩汁10%、罗汉果苷甜味成分1%。其中罗汉果苷V含量3.97%(以该组合物总质量为计算基准;罗汉果苷V含量超过所述罗汉果苷甜味成分,原因也如前所述,是因为罗汉果芳香挥发油、甜香脱色浓缩汁和纯味脱色浓缩汁中也含有部分罗汉果苷V),稀释或溶解的水溶液(固体含量1%w/v)在420nm处的吸光度0.02。
本实施例的气相色谱图和高效液相色谱图分别如图4和图8所示。
二、本发明罗汉果苷甜味和风味组合物各组分的制备方法实施例
本发明罗汉果苷甜味和风味组合物的制备方法实施例,包括以下步骤:
I、罗汉果芳香挥发油收集
(1)糖化后熟:用罗汉果专用量果板将鲜罗汉果按大、中、小、外果分类,然后按类用罗汉果专用筐装好,层堆在室内通风阴凉处,堆3层,中途每3天翻动一次,让其水分自然蒸发和促进内部糖分的转化;在室内放置8天,至果实表面有50%呈现黄色,水分蒸发失重占果重的12%,即罗汉果果皮呈现绿豆黄时,分别进入烤房烘烤;
(2)烤房烘烤与芳香挥发油收集:将糖化后熟的罗汉果果实,按照大、中、小、外果分别装入网盘,点火升温,在烘烤过程中,温度由低温逐步升至高温再降温,分为三个过程:
第一阶段,逐步升温至47℃,维持2天,使罗汉果中水分逐步蒸发,让水蒸气排出;
第二阶段,逐步提高到66℃,持续3天,使罗汉果中水分加快蒸发;
第三阶段,降温到56℃,继续烘烤2天,使果实的重量下降到相当鲜果重量的28%,停火,自然降温,出炉;
在罗汉果烘烤过程中,罗汉果所含芳香挥发油随同水分一并逐步挥发、蒸发,经冷却,形成芳香挥发油和水的混合物,通过烤房所设芳香挥发油收集装置予以收集,得罗汉果芳 香挥发油;烘烤完毕,还得罗汉果干果;
II、甜香脱色浓缩汁提取精制
(1)糖化后熟:用罗汉果专用量果板将新鲜成熟的罗汉果按大、中、小、外果分类,然后按类用罗汉果专用筐装好,层堆在室内通风阴凉处,堆3层,中途每3天翻动一次,让其水分自然蒸发和促进内部糖分的转化;在室内放置7天,至果实表面有50%呈现黄色,水分蒸发失重占果重的10%,即罗汉果果皮呈现绿豆黄时,剥去外皮后分别进入去皮果专用烤箱烘烤;
(2)烤箱烘烤和与芳香挥发油收集:将糖化后熟的罗汉果果实,按照大、中、小、外果分类,剥去果皮,铺摊成厚度约0.6~1.0cm,再分别装入网盘,用去皮果烤箱烘烤;在烘烤过程中,温度及时间控制如下:
第一阶段,升温到82℃,维持5h;
第二阶段,降温到73℃,持续20h;
第三阶段,降温到62℃,继续烘烤35h,使果实的重量下降到相当去皮果的25%,表面呈深黄色至黄褐色,并具有浓郁的果香味和焦香味时,断电,自然降温,出箱;
在去皮果烘烤过程中,同时利用芳香挥发油收集装置收集具有浓郁果香味和焦香味的去皮果芳香挥发油;
(3)甜香脱色浓缩汁提取、精制
A.提取
用提取罐提取,按以下步骤操作:
将去皮罗汉果干果400kg投入6m 3提取罐中,加纯化水提取,提取温度85℃;开启搅拌器;提取3次;每次提取时间分别为2.0、1.5、1.0h;加入纯化水的量分别是3600L、3200L、2400L,第3次用作套提液,进入下批物料;每次提取完后,过滤,滤渣进入下一次提取,提完第三次后,滤渣另行处理;合并3次提取液,得提取罐提取液约6000L;
B.离心过滤与陶瓷膜澄清
先用离心去除较粗颗粒杂质,再通过陶瓷膜成套设备去除细小杂质,最终得到澄清透明的滤液;离心方法如下:
a卧螺离心:将提取罐提取液通过卧螺离心机过滤,得卧螺滤液;
b碟式离心:将卧螺滤液通过碟式离心过滤,得碟式滤液;
c陶瓷膜澄清:将碟式滤液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.45μm,材质为氧化铝,得澄清透明的陶瓷膜滤液;
C.膜分离与浓缩
将陶瓷膜滤液冷却至42℃,然后进行脱色、浓缩:
a超滤脱色:将冷却好的陶瓷膜滤液通过超滤膜成套设备脱色,选择超滤膜孔径8KD,收集膜下游液即脱色液,得膜脱色液;
b反渗透膜浓缩:将膜脱色液通过反渗透膜成套设备浓缩至8Brix,得1600L膜浓缩液;
D.树脂脱色
通过阴离子树脂和阳离子树脂进一步脱色,以得到接近无色的脱色液:
a阴离子树脂:阴离子树脂柱装D900型阴离子树脂200kg;将膜浓缩液通过阴离子树脂脱色,进完料以后,再用600L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阴离子树脂脱色液;
b阳离子树脂:阳离子树脂柱装D717阳离子树脂160kg。将阴离子树脂脱色液通过阳离子树脂脱盐,进完料以后,再用480L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得阳离子树脂脱盐液;
E.树脂脱苦、脱农残、脱重金属
通过专用树脂进一步脱苦、脱农残、脱重金属,以得到口感、农残、重金属合格的优质产品;
a脱苦:脱苦专用树脂柱装LSA-600树脂120kg;将阳离子树脂脱盐液通过脱苦专用树脂脱苦,进完料以后,再用360L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得脱盐脱苦液;
b脱农残:脱农残专用树脂柱装LSA-900树脂120kg;将脱苦脱盐液通过脱农残专用树脂脱农残,进完料以后,再用360L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱盐脱苦脱农残液;
c脱重金属:脱重金属专用树脂柱装LSC-400树脂120kg;将脱农残液通过脱重金属专用树脂脱重金属,进完料以后,再用360L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得3700L脱盐脱苦脱农残脱重金属液;
F.活性炭去异味
活性炭柱装粒状活性炭8kg;
预先将活性炭装于层析柱内,然后将脱重金属液通过活性炭柱去异味,进完料以后,再用24L纯化水洗柱;合并流出液和水洗液,板框过滤,得脱盐脱苦脱农残脱重金属去异味液;
G.陶瓷膜澄清
将去异味液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.22μm,材质为氧化铝,得澄清透明的脱盐脱苦脱农残脱重金属陶瓷膜滤液;
H.真空浓缩
将脱盐脱苦脱农残脱重金属陶瓷膜滤液进行真空浓缩,控制温度≤65℃,真空度≥0.085MPa,浓缩至65Brix,得130kg脱盐脱苦脱农残脱重金属的甜香脱色浓缩汁;
经HPLC检测,罗汉果苷V含量3.26%;
III、纯味脱色浓缩汁提取精制
(1)糖化后熟:用罗汉果专用量果板将新鲜成熟的罗汉果按大、中、小、外果分类,然后按类用罗汉果专用筐装好,层堆在室内通风阴凉处,可堆3层,中途每3天翻动一次,让其水分自然蒸发和促进内部糖分的转化。在室内放置9天,至果实表面有50%呈现黄色,水分蒸发失重占果重的14%,即罗汉果果皮呈现绿豆黄时,即可进入提取纯味脱色浓缩汁工序。
(2)提取
将糖化后熟的罗汉果通过与逆流提取槽相连的罗汉果专用破碎机破碎后进入逆流提取工序,按以下操作:
将破碎好的罗汉果20 000kg投入逆流提取槽中,用纯化水提取;提取温度90℃;提取方式:动态连续逆流提取;提取时间2.0h;纯化水加入体积量为罗汉果重量的2.0倍,即40 000L(纯化水体积/鲜罗汉果重量,V/W);提取完后过滤,滤渣另行处理;合并不断流出的提取液,得39000L逆流提取液;
(3)离心过滤与陶瓷膜澄清
先用离心去除大部分较粗颗粒杂质,再通过陶瓷膜成套设备去除细小杂质,最终得到澄清透明的滤液;
a卧螺离心:将提取罐提取液或逆流提取液通过卧螺离心机过滤,得卧螺滤液;
b碟式离心:将卧螺滤液通过碟式离心过滤,得碟式滤液;
c陶瓷膜澄清:将碟式滤液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.45μm,材质为氧化铝,得澄清透明的陶瓷膜滤液;
(4)膜分离与浓缩
将陶瓷膜滤液冷却至45℃;
a超滤脱色:将冷却好的陶瓷膜滤液通过超滤膜成套设备脱色,选择超滤膜孔径10KD,收集膜下游液即脱色液,得膜脱色液;
b反渗透膜浓缩:将膜脱色液通过反渗透膜成套设备浓缩至10Brix,得22 000L膜浓 缩液;
(5)树脂脱色
通过阴离子树脂和阳离子树脂进一步脱色,以得到接近无色的脱色液;
a阴离子树脂:阴离子树脂柱装D941型阴离子树脂2200kg;将膜浓缩液通过阴离子树脂脱色,进完料以后,再用6600L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得阴离子树脂脱色液;
b阳离子树脂:阳离子树脂柱装D717阳离子树脂1800kg;将阴离子树脂脱色液通过阳离子树脂脱盐,进完料以后,再用5400L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得阳离子树脂脱盐液;
(6)树脂脱苦、脱农残、脱重金属
通过专用树脂进一步脱苦、脱农残、脱重金属,以得到口感好、农残、重金属含量达标的优质产品;
a脱苦:脱苦专用树脂柱装LSA-600树脂1600kg。将阳离子树脂脱盐液通过脱苦专用树脂脱苦,进完料以后,再用4800L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得脱苦脱色脱盐液;
b脱农残:脱农残专用树脂柱装LSA-900树脂1600kg。将脱苦脱色脱盐液通过脱农残专用树脂脱农残,进完料以后,再用4800L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得脱农残脱苦脱色脱盐液;
c脱重金属:脱重金属专用树脂柱装LSC-400树脂1600kg。将脱农残脱苦脱色脱盐液通过脱重金属专用树脂脱重金属,进完料以后,再用4800L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得48500L脱重金属脱农残脱苦脱色脱盐液;
(7)活性炭去异味
活性炭柱装粒状活性炭80kg;
预先将活性炭装于层析柱内,然后将脱重金属液通过活性炭柱去异味,进完料以后,再用240L纯化水洗柱;合并流出液和水洗液,板框过滤,得去异味脱重金属脱农残脱苦脱色脱盐液;
(8)陶瓷膜澄清
将去异味脱重金属脱农残脱苦脱色脱盐液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.22μm,材质为氧化铝,得澄清透明的陶瓷膜滤液;
(9)真空浓缩
将陶瓷膜滤液真空浓缩,控制温度≤65℃,真空≥0.085MPa,浓缩至60Brix,得2950kg 脱重金属脱农残脱苦脱色脱盐的纯味脱色浓缩汁;
经HPLC检测,罗汉果苷V含量3.82%;
IV、罗汉果苷等甜味成分提取;
(1)糖化后熟:用罗汉果专用量果板将新鲜成熟的罗汉果按大、中、小、外果分类,然后按类用罗汉果专用筐装好,层堆在室内通风阴凉处,堆4层,中途每3天翻动一次,让其水分自然蒸发和促进内部糖分的转化;在室内放置8天,至果实表面有50%呈现黄色,水分蒸发失重占果重的13%,即罗汉果果皮呈现绿豆黄时,进入提取罗汉果苷等甜味成分工序;
(2)提取
将糖化后熟的罗汉果通过与逆流提取槽相连的罗汉果专用破碎机破碎后进入逆流提取工序,按以下操作:
将破碎好的罗汉果10 000kg投入逆流提取槽中,用纯化水提取;提取温度:85℃;提取方式:动态连续逆流提取;提取时间:2.0h;纯化水加入量为罗汉果重量的2.0倍,即20 000L(纯化水体积/鲜罗汉果,V/W);提取完后过滤,滤渣另行处理;合并不断流出的提取液,得20 000L逆流提取液;
(3)离心过滤与陶瓷膜澄清
先用离心去除大部分机械杂质,再通过陶瓷膜成套设备去除细小杂质,最终得到澄清透明的滤液;
a卧螺离心:将提取罐提取液或逆流提取液通过卧螺离心机过滤,得卧螺滤液;
b碟式离心:将卧螺滤液通过碟式离心过滤,得碟式滤液;
c陶瓷膜澄清:将碟式滤液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.45μm,材质为氧化锆,得澄清透明的陶瓷膜滤液;
(4)膜分离精制
所述膜为超滤膜;将陶瓷膜滤液通水冷却至40℃;
a大分子量超滤精制:将冷却好的陶瓷膜滤液通过大分子量超滤膜成套设备精制,选择超滤膜孔径8KD,收集膜下游液即精制液,得大分子量超滤膜精制液;
b小分子量超滤精制及浓缩:将大分子量超滤膜精制液通过小分子量超滤膜成套设备精制,选择超滤膜孔径2KD,收集膜上游液即精制液,得11000L小分子量超滤膜精制液;
(5)树脂脱色
通过阴离子树脂和阳离子树脂进一步脱色,以得到接近无色的脱色液;
a阴离子树脂:阴离子树脂柱装D941型阴离子树脂1000kg;将膜浓缩液通过阴离子 树脂脱色,进完料以后,再用3000L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阴离子树脂脱色液;
b阳离子树脂:阳离子树脂柱装001×16阳离子树脂850kg;将阴离子树脂脱色液通过阳离子树脂脱盐,进完料以后,再用2500L纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得阳离子树脂脱盐的脱色液;
(6)树脂脱苦、脱农残、脱重金属
通过专用树脂进一步脱苦、脱农残、脱重金属,以得到口感好、农残、重金属含量达标的优质产品;
a脱苦:脱苦专用树脂柱装LSA-600树脂750kg;将阳离子树脂脱盐的脱色液通过脱苦专用树脂脱苦,进完料以后,再用2250L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱苦脱盐脱色液;
b脱农残:脱农残专用树脂柱装LSA-900树脂750kg。将脱苦脱盐脱色液通过脱农残专用树脂脱农残,进完料以后,再用2250L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱农残脱苦脱盐脱色液;
c脱重金属:脱重金属专用树脂柱装LSC-400树脂750kg;将脱农残脱苦脱盐脱色液通过脱重金属专用树脂脱重金属,进完料以后,再用2250L纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得23250L脱重金属脱农残脱苦脱盐脱色液;
(7)活性炭去脱异味
活性炭柱装粒状活性炭45kg;
预先将活性炭装于层析柱内,然后将脱重金属脱农残脱苦脱盐脱色液通过活性炭柱去异味,进完料以后,再用300L纯化水洗柱;合并流出液和水洗液,板框过滤,得去异味脱重金属脱农残脱苦脱盐脱色液;
(8)陶瓷膜澄清
将去异味脱重金属脱农残脱苦脱盐脱色液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.22um,材质为氧化铝或氧化锆,得去异味脱重金属脱农残脱苦脱盐脱色的液澄清透明的陶瓷膜滤液;
(9)膜分离脱味与浓缩
所述膜为纳滤膜;
将所述陶瓷膜滤液通过纳滤膜成套设备,浓缩至8Brix,去除小分子物质和杂味,并浓缩,得到2100L纳滤膜精制液;
(10)真空浓缩
将所述纳滤膜精制液进行真空浓缩,控制温度≤65℃,真空≥0.085MPa,浓缩至20°波美,得真空浓缩液;
(11)干燥
将真空浓缩液喷雾干燥得成品-罗汉果苷甜味成分,产品重量165kg;
经HPLC检测,罗汉果苷V含量36.15%;
(V)罗汉果苷甜味和风味组合物混配:将步骤I所得罗汉果芳香挥发油、步骤II所得甜香脱色浓缩汁、步骤III所得纯味脱色浓缩汁、步骤IV所得罗汉果苷甜味成分,根据口感、气味、甜度持久性、产品存在形式要求,进行混配,即得罗汉果苷甜味和风味组合物。
具体参见第一部分本发明罗汉果苷甜味和风味组合物实施例的实施例1、实施例2、实施例3、实施例4。

Claims (10)

  1. 罗汉果苷甜味和风味组合物,其特征在于,包括有罗汉果芳香挥发油、罗汉果甜香脱色浓缩汁、罗汉果纯味脱色浓缩汁及罗汉果苷甜味成分中的至少一种,其中甜香脱色浓缩汁、纯味脱色浓缩汁和罗汉果苷甜味成分≠0。
  2. 根据权利要求1所述的罗汉果苷甜味和风味组合物,其特征在于,以所述罗汉果苷甜味和风味组合物的总质量为计算基准,罗汉果苷V的质量含量为1%~15%。
  3. 根据权利要求1或2所述的罗汉果苷甜味和风味组合物,其特征在于,含有罗汉果挥发油成分n-十六烷酸或/和9,12-十八碳二烯酸,或无籽罗汉果挥发油成分乙二醇异丙醚、1,2-苯二甲酸丁基-2-乙基己酯、邻苯二甲酸二异丁酯、天竺葵醛中的一种,或所述几种挥发油成分的组合,所述罗汉果挥发油的总质量含量为0%~5%;优选0.5%~4.0%。
  4. 一种如权利要求1-3之一所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,包括以下步骤:(I)罗汉果芳香挥发油收集;(II)罗汉果甜香脱色浓缩汁的提取精制;(III)罗汉果纯味脱色浓缩汁的提取精制;(IV)罗汉果苷甜味成分的提取精制;(V)混配。
  5. 根据权利要求4所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,步骤(I)中,所述罗汉果芳香挥发油收集的方法是:
    (1)糖化后熟:将鲜罗汉果用筐装好,层堆在室内通风阴凉处,让罗汉果中的水分自然蒸发,促进内部糖分的转化,至罗汉果果皮呈现绿豆黄色;
    优选方案:对鲜罗汉果按大、中、小、外果进行分类,然后按类分别用罗汉果专用筐装好,再进行层堆;层堆的层数为2~4层,在室内放置天数为7~10天,中间每隔3~4天翻动一次;至果实表面有≥50%面积呈现黄色,水分蒸发失重占鲜果重量的10~15%;
    进一步的优选方案:用罗汉果专用量果板对鲜罗汉果按大、中、小、外果进行分类;
    (2)烤房烘烤与芳香挥发油收集:将经步骤(1)糖化后熟的罗汉果果实,装入网盘,然后置于设有芳香挥发油收集装置的烤房的网盘放置架上,点火升温烘烤;
    在罗汉果烘烤过程中,罗汉果所含芳香挥发油会随同罗汉果所含水分一起逐步挥发、蒸发,经冷却,形成芳香挥发油和水的混合物,通过烤房所设芳香挥发油收集装置予以收集,得罗汉果芳香挥发油;烘烤完毕,还得罗汉果干果;
    装网盘优选方案:按照大、中、小、外果类别,分别装入网盘;
    烘烤方法优选方案:在烘烤过程中,烘烤的升温降温过程,分为以下三个阶段:
    第一阶段:升温至45℃~50℃,维持2~3天,使罗汉果中的水分和芳香挥发油逐步排出、蒸发、挥发;
    第二阶段:逐步提高温度至65℃~70℃,持续2~3天,使水分和芳香挥发油加快排出、蒸发、挥发;
    第三阶段:逐步降温至55℃~60℃,继续烘烤,使果实的重量下降到相当鲜果的25~30%,然后停火,自然降温至环境温度,出炉;
    所述芳香挥发油收集装置结构优选方案:采用以下构件构成:包括不锈钢导管,所述不锈钢导管的首端与烤房顶部的排气孔连接,不锈钢导管的尾端伸出烤房之外,伸出烤房之外的不锈钢导管的管壁外侧设有冷却装置,不锈钢导管的尾端出口处设有接收芳香挥发油与水混合物的芳香挥发油收集储罐,所述芳香挥发油收集储罐侧壁设有用于观察收集储罐内液位的液位指示器。
  6. 根据权利要求4或5所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,步骤(II)中,所述甜香脱色浓缩汁的提取精制方法包括以下步骤:糖化后熟;专用烤箱去皮烘烤;提取;离心过滤与陶瓷膜澄清;膜分离与浓缩;树脂脱色;树脂脱苦、脱农残、脱重金属;活性炭去异味;陶瓷膜澄清;真空浓缩;
    优选方案:
    (1)糖化后熟:操作方法同步骤(I)的(1)糖化后熟;
    (2)烤箱烘烤与芳香挥发油收集:将糖化后熟的罗汉果果实,剥去果皮,铺摊成片状或块状,再分别装入网盘,用烤箱烘烤,得去皮罗汉果干果;
    在烘烤过程中,去皮罗汉果所含芳香挥发油会随同水分逐步同时挥发、蒸发,经冷却,形成芳香挥发油和水的混合物,通过所设芳香挥发油收集装置予以收集,得罗汉果芳香挥发油;
    铺摊优选方案:按照大、中、小、外果分类,进行铺摊;
    烘烤方法优选方案:在烘烤过程中,烘烤的升温降温过程,分为以下三个阶段:
    第一阶段:升温到80℃~85℃,维持4~8h;
    第二阶段:降温到75℃~70℃,持续16~24h;
    第三阶段:降温到65℃~60℃,继续烘烤30~40h,使果实的重量下降到相当去皮果重量的20~30%,表面呈深黄色至黄褐色,并具有浓郁的果香味和焦香味时,停止烘烤,自然降温,出箱;
    芳香挥发油收集装置优选方案:采用以下构件构成:包括不锈钢导管,所述不锈钢导管的首端与烤箱顶部的排气孔连接,不锈钢导管的尾端伸出烤房之外,伸出烤房之外的不锈钢导管的管壁外侧设有冷却装置,不锈钢导管的尾端出口处设有接收芳香挥发油和水混合物的芳香挥发油收集储罐;所述芳香挥发油收集储罐侧壁设有用于观察收集储罐内液位 的液位指示器;
    (3)甜香脱色浓缩汁的提取、精制:
    A.提取
    采用提取罐提取或逆流提取槽提取:
    a)提取罐提取:将步骤(II)的步骤(2)所得去皮罗汉果干果投入提取罐中,加水搅拌,再进行固液分离,得提取罐提取液;
    优选方案:所述水为纯化水;提取温度优选80℃~95℃;提取次数3次,每次提取时间分别为1.5~2.5h、1.0~2.0h、0.5~1.5h;每次纯化水加入体积量分别为去皮罗汉果干果重量的8~10倍、7~9倍、5~7倍;每次提取完成后,过滤,滤渣进入下一次提取,第三次提取完成后,滤渣另行处理;合并3次提取液,即得提取罐提取液;
    b)逆流提取槽提取:将步骤(II)的步骤(2)所得去皮罗汉果干果投入逆流提取槽中,加水进行逆流提取;
    优选方案:所述水为纯化水;提取温度优选80℃~95℃;提取时间1.5-2.5h;纯化水加入体积量为去皮罗汉果干果重量的4~6倍(纯化水体积/干燥的去皮果,V/W);提取完成后,过滤,滤渣另行处理;合并不断流出的提取液,得逆流提取槽提取液;
    B.离心过滤与陶瓷膜澄清
    先离心,去除提取罐提取液或逆流提取槽提取液中的较粗颗粒杂质,再通过陶瓷膜成套设备去除其中的细微杂质,最终得到澄清透明的滤液;
    优选方案:
    a)卧螺离心:将提取罐提取液或逆流提取槽提取液通过卧螺离心机过滤,得卧螺离心滤液;
    b)碟式离心:将卧螺滤液通过碟式离心过滤,得碟式离心滤液;
    c)陶瓷膜澄清:将碟式滤液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.45μm,材质为氧化铝或氧化锆,得澄清透明的陶瓷膜滤液;
    C.膜分离与浓缩
    将陶瓷膜滤液通过水冷却,再用超滤膜通过膜分离去除大部分色素,然后用反渗透膜浓缩,方便脱色及后续操作;
    优选方案:
    a)将陶瓷膜滤液通过水冷却至45℃以下;
    b)超滤脱色:将冷却好的陶瓷膜滤液通过超滤膜成套设备脱色,选择超滤膜孔径8KD~10KD,收集膜下游液即脱色液,得膜脱色液;
    c)反渗透膜浓缩:将膜脱色液通过反渗透膜成套设备浓缩至5~10Brix,得膜浓缩液;
    D.树脂脱色
    通过阴离子树脂和阳离子树脂脱色,以得到接近无色的脱色液;
    优选方案:所述阴离子树脂包括凝胶型及大孔型丙烯酸弱碱阴离子树脂、丙烯酸系强碱和弱碱阴离子树脂、凝胶型及大孔型苯乙烯系强碱阴离子树脂、大孔型丙烯酸强碱阴离子树脂、大孔型苯乙烯系弱碱阴离子树脂;
    所述阳离子树脂包括凝胶型及大孔型苯乙烯系强酸阳离子树脂、丙烯酸系凝胶型和大孔型弱酸阳离子树脂;
    阴离子树脂优选型号:D900、D941、D316、D296;
    阳离子树脂优选型号:001×16,D717;
    进一步的优选方案:
    a)阴离子树脂用量为:每1000kg去皮罗汉果干果用350kg~5500kg;将膜浓缩液通过阴离子树脂脱色,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阴离子树脂脱色液;
    b)阳离子树脂用量为:每1000kg去皮罗汉果干果用250kg~450kg;将阴离子树脂脱色液通过阳离子树脂脱盐,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得阳离子树脂脱盐液;
    E.树脂脱苦、脱农残、脱重金属
    通过树脂进一步脱苦、脱农残、脱重金属,使之口感良好,农残、重金属含量达标;
    优选方案:所述脱苦、脱农残、脱重金属所用树脂包括凝胶型及大孔型丙烯酸树脂、丙烯酸系树脂、凝胶型及大孔型苯乙烯系树脂、大孔型丙烯酸树脂、大孔型苯乙烯系树脂、丙烯酸系凝胶型树脂;
    脱苦专用树脂优选型号:LSA-600、LX-900;
    脱农残专用树脂优选型号:LSA-900B、LSA-900D;
    脱重金属专用树脂优选型号:LX-500、LSC-As、LSC-400;
    进一步的优选方案:
    a)使用脱苦专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将阳离子树脂脱盐液通过脱苦专用树脂柱脱苦,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出。合并流出液及水洗液,得脱苦液;
    b)使用脱农残专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将脱苦液通过脱农残专用树脂柱脱农残,进完料以后,再用纯化水洗柱,将柱内残存的有效成分 洗出;合并流出液及水洗液,得脱苦脱农残液;
    c)使用脱重金属专用树脂,用量为每1000kg去皮罗汉果干果用250kg~350kg;将脱苦脱农残液通过脱重金属专用树脂柱脱重金属,进完料以后,再用纯化水洗柱,将柱内残存的有效成分洗出;合并流出液及水洗液,得脱苦脱农残脱重金属液;
    F.活性炭去异味
    活性炭用量为,每1000kg去皮罗汉果干果用活性炭12kg~20kg;所述活性炭为粒状活性炭;
    优选方案:预先将活性炭装于层析柱内,然后将脱苦脱农残脱重金属液通过活性炭柱去异味,进完料以后,再用纯化水洗柱;合并流出液和水洗液,板框过滤,得脱苦脱农残脱重金属去异味液;
    G.陶瓷膜澄清
    将脱苦脱农残脱重金属去异味液通过陶瓷膜成套设备澄清,其中陶瓷膜孔径0.22μm,材质为氧化铝或氧化锆,得澄清透明的陶瓷膜滤液;
    H.真空浓缩
    将陶瓷膜滤液真空浓缩,控制温度≤65℃,真空度≥0.085MPa,浓缩至60~70Brix,即得甜香脱色浓缩汁。
  7. 根据权利要求4~6之一所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,步骤(III)中,所述纯味脱色浓缩汁提取精制的方法包括以下步骤:以新鲜成熟的罗汉果为原料,糖化后熟;再用提取罐提取或逆流提取槽提取;离心与陶瓷膜澄清;膜分离与浓缩;树脂脱色;树脂脱苦、脱农残、脱重金属;活性炭去异味;陶瓷膜澄清;真空浓缩;
    优选方案:
    (1)糖化后熟:同步骤(I)的(1)糖化后熟;
    (2)提取
    将糖化后熟的罗汉果通过破碎机破碎后进入提取工序;
    优选方案:
    a)提取罐提取:基本同步骤(II)的(3)甜香脱色浓缩汁A.提取项下a)提取罐提取,所不同的是此处原料是鲜罗汉果,且纯化水加入体积量分别为罗汉果质量的2~4倍、2~4倍、2~3倍;
    b)逆流提取槽提取:同步骤(II)的(3)甜香脱色浓缩汁A.提取项下b)逆流提取槽提取,所不同的是纯化水加入体积量为鲜罗汉果质量的1.2~2.0倍;
    (3)离心过滤与陶瓷膜澄清
    操作方法同步骤(II)的(3)甜香脱色浓缩汁B.离心过滤与陶瓷膜澄清;
    (4)膜分离与浓缩
    操作方法同步骤(II)的(3)甜香脱色浓缩汁C.膜分离与浓缩;
    (5)树脂脱色
    操作方法基本同步骤(II)的(3)甜香脱色浓缩汁D.树脂脱色,所不同的是
    更优选的方案:
    a)阴离子树脂:阴离子树脂用量为每1000kg鲜罗汉果用阴离子树脂90kg~150kg;
    b)阳离子树脂:阳离子树脂用量为每1000kg鲜罗汉用60kg~120kg;
    (6)树脂脱苦、脱农残、脱重金属
    操作方法基本同步骤(II)的(3)甜香脱色浓缩汁E.树脂脱苦、脱农残、脱重金属,所不同的是
    更优选的方案:
    a)脱苦:用量为每1000kg鲜罗汉果用树脂60kg~90kg;
    b)脱农残:用量为每1000kg鲜罗汉果用树脂60kg~90kg;
    c)脱重金属:用量为每1000kg鲜罗汉果用树脂60kg~90kg;
    (7)活性炭去异味
    操作方法基本同步骤(II)的(3)甜香脱色浓缩汁F.活性炭去异味,所不同的是活性炭用量为,每1000kg鲜罗汉果用活性炭3~5kg;
    (8)陶瓷膜澄清
    同步骤(II)的(3)甜香脱色浓缩汁G.陶瓷膜澄清;
    (9)真空浓缩
    同步骤(II)的(3)甜香脱色浓缩汁H.真空浓缩;
  8. 根据权利要求5~7之一所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,步骤(IV)中,所述罗汉果苷甜味成分的提取精制方法,包括以下步骤,将新鲜成熟的罗汉果糖化后熟,提取罐或逆流提取槽提取,离心过滤与陶瓷膜澄清,膜分离精制,树脂脱色,树脂脱苦、脱农残、脱重金属,活性炭去农残及脱异味,陶瓷膜澄清,膜分离脱杂味,真空浓缩,干燥;
    优选方案:
    (1)糖化后熟:同步骤(I)的(1)糖化后熟;
    (2)提取
    a)提取罐提取:同步骤(III)的(2)提取a)提取罐提取;
    b)逆流提取槽提取:同步骤(III)的(2)提取b)逆流提取槽提取;
    (3)离心过滤与陶瓷膜澄清
    同步骤(III)的(3)离心过滤与陶瓷膜澄清;
    (4)膜分离精制
    所述膜为超滤膜;将陶瓷膜滤液通水冷却,根据罗汉果苷甜味成分分子分量大小差异,先用大分子量的超滤膜进行分子截留,去除大部分色素和杂质,再用小分子量的超滤膜进行分子截留,收集罗汉果苷甜味成分;
    优选方案:
    a)大分子量超滤精制:将冷却至45℃以下的陶瓷膜滤液,通过大分子量超滤膜成套设备精制,选择超滤膜孔径8KD~10KD,收集膜下游液即精制液,得大分子量超滤膜精制液;
    b)小分子量超滤精制及浓缩:将大分子量超滤膜精制液通过小分子量超滤膜成套设备精制,选择超滤膜孔径2KD~3KD,收集膜上游液即精制液,得小分子量超滤膜精制液;
    (5)树脂脱色
    同步骤(III)的(5)树脂脱色;
    (6)树脂脱苦、脱农残、脱重金属
    同步骤(III)的(6)树脂脱苦、脱农残、脱重金属;
    (7)活性炭去农残及脱异味
    同步骤(III)的(7)活性炭去异味;
    (8)陶瓷膜澄清
    同步骤(III)的(8)陶瓷膜澄清;
    (9)膜分离脱杂味
    优选方案:
    所述膜为纳滤膜;
    将陶瓷膜滤液通过纳滤膜成套设备,浓缩至原体积1/4,去除小分子物质和杂味;
    (10)真空浓缩
    优选方案:
    将膜分离液真空浓缩,控制温度≤65℃,真空度≥0.085MPa,浓缩至17~25波美,得真空浓缩液;
    (11)干燥
    将真空浓缩液喷雾干燥或微波真空干燥,得罗汉果苷甜味成分产品。
  9. 根据权利要求5-8之一所述的罗汉果苷甜味和风味组合物的制备方法,其特征在于,步骤(V),所述混配是指,将收集的烘焙罗汉果的芳香挥发油、提取精制的甜香脱色浓缩汁、纯味脱色浓缩汁、罗汉果苷甜味成分,根据口感、气味、甜度持久性、产品存在形式要求,进行混配。
  10. 根据权利要求1-3之一所述的罗汉果苷甜味和风味组合物在食品、饮品、乳品、保健品和药品中的应用。
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