WO2023213325A1 - 一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法 - Google Patents

一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法 Download PDF

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WO2023213325A1
WO2023213325A1 PCT/CN2023/092553 CN2023092553W WO2023213325A1 WO 2023213325 A1 WO2023213325 A1 WO 2023213325A1 CN 2023092553 W CN2023092553 W CN 2023092553W WO 2023213325 A1 WO2023213325 A1 WO 2023213325A1
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octacosanol
purity
deuterated water
flavonoids
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PCT/CN2023/092553
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French (fr)
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谭卓华
黄炜岚
谭晓露
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广州绿徽新材料研究院有限公司
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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
    • A23L2/38Other 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
    • 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
    • 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
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • 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
    • A23L33/125Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
    • 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
    • A23L33/20Reducing nutritive value; Dietetic products with reduced nutritive value
    • A23L33/21Addition of substantially indigestible substances, e.g. dietary fibres
    • 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

Definitions

  • the invention relates to the technical field of food processing, and specifically designs a high-energy beverage that is synergistically refined with an ultra-high-purity octacosanol-flavonoid composite deuterated water combination and a preparation method thereof.
  • 1.Octacosanol is a natural higher fatty alcohol with good biodegradability and easy to be absorbed by the human body.
  • octacosanol has the function of lowering blood lipids.
  • Qi Xiaoming and others proposed that the hypolipidemia effect of octacosanol is related to the dosage. Higher dosages of this substance can significantly reduce the TG, TC and LDL-C content in the serum; while low dosages only have an effect on the serum lipid levels.
  • TC concentration has an impact.
  • Research by DevK.Singh et al. proposed that octacosanol reduces cholesterol content in serum by activating enzyme activity through phosphorylation of AMP-kinase, thereby reducing HMG-CoA enzyme activity and controlling cholesterol synthesis in serum. Purpose;
  • Octacosanol can reduce excess calcium and fat content in the blood and is a promoter of calcitonin formation.
  • octacosanol is known as a compound that can relieve physical fatigue and has good biological activity. Research shows that this substance can improve the human body's endurance, quickly restore physical strength, and improve related physiological indicators in body fluids after activity;
  • octacosanol has a very small dosage but significant physiological activity. It can quickly eliminate fatigue and enhance physical strength and endurance. It is a world-recognized anti-fatigue functional substance. According to reports from Nippon Oils and Fats Co., Ltd., usually 0.2 mg of octacosanol is taken orally per person per day to eliminate fatigue; in order to enhance physical strength and endurance, the daily oral dosage is about 0.5 mg; and for therapeutic purposes The dosage is 5mg;
  • bamboo leaf flavonoids are a type of plant flavonoids, and the active ingredients are flavonoid glycosides and coumarin lactones. In addition to flavonoids, its components also include phenolic acids, anthraquinones, aromatic components, and trace elements such as manganese, zinc, and tin. Together, they form the basis for the extensive physiological and pharmacological activities of bamboo leaf flavonoids.
  • It has the functions of scavenging oxygen free radicals, resisting aging, preventing Alzheimer's disease, preventing vascular sclerosis, resisting vascular proliferation, resisting myocardial ischemia, lowering blood pressure, lowering blood lipids, and protecting cardiovascular and cerebrovascular diseases. It can be used to prevent and treat cardiovascular and cerebrovascular diseases. If it can reduce The fragility of blood vessels, dilating blood vessels and improving blood vessel permeability, preventing arteriosclerosis, lowering blood lipids and cholesterol, preventing and treating hypertension in the elderly, cerebral hemorrhage, coronary heart disease, angina pectoris, dilating coronary blood vessels, increasing coronary flow, lowering blood sugar, etc. good effect;
  • liver protection liver detoxification, treatment of acute and chronic hepatitis, liver cirrhosis, improvement of body immunity, diarrhea, cough relieving, expectoration, asthma, antispasmodic, anti-allergic, anti-allergic and anti-viral, etc. pharmacological effects;
  • Oxidative stress has been shown to contribute to chronic fatigue through increased release of pro-inflammatory cytokines such as tumor necrosis factor- ⁇ (TNF- ⁇ ), interleukin-6 (IL-6), and IL-1 ⁇ ;
  • TNF- ⁇ tumor necrosis factor- ⁇
  • IL-6 interleukin-6
  • IL-1 ⁇ pro-inflammatory cytokines
  • LN lutein-6-c-neohesperidin luteolin-6-c-neohesperidin
  • bamboo leaf flavonoids can prevent or delay the oxidation of food, improve the stability of food and extend the storage period;
  • the current main raw materials for extracting octacosanol are sugarcane, bran wax, insecticide, and wheat germ oil, it is insoluble in water and soluble in organic solvents.
  • the structure of the existing substance is relatively complex. Therefore, how to extract it from natural substances? Efficient, economical and environmentally friendly extraction is a problem that should be solved in the production of a large amount of high-quality such substances.
  • the raw materials are saponified and extracted with organic solvents (n-hexane, acetone, etc.), a A white or light yellow powdery product.
  • This powdery crystal is a natural high-grade alkanol mixture (containing higher alkanols with 24-34 carbon atoms).
  • the content of octadecane in this mixture is 50-70%. , and the relevant pharmacological experiments in the data were also conducted on extracts with this content.
  • the product technology is only that the conventional extraction purity of octacosanol can only reach 40-80%, such as: a sports drink and its manufacturing method - 200510036559.0 (no rights - no annual fee paid) claim 5.
  • the sports drink is characterized in that: the purity of the octacosanol used is greater than 80% .
  • wheat germ beverage and its preparation method-201010615889.6 no rights-unpaid annual fee
  • the described octacosanol is first extracted from wheat germ using a supercritical CO2 extraction method to obtain white flake crystals of octacosanol, in which the octacosanol content is 42.1 to 43.5% ;
  • Flavonoids have very different solubility properties due to their different structures and sources. Therefore, appropriate solvents should be selected for extraction based on their polarity and water solubility. With the continuous deepening of research, there are more and more extraction methods for bamboo leaf flavonoids. According to the literature, the common extraction methods of bamboo flavonoids include hot water extraction, organic solvent extraction, microwave extraction, ultrasonic extraction, Supercritical fluid extraction, enzyme extraction, crushing extraction and other methods;
  • the extracts obtained by the above-mentioned single methods have good stability in the pH range of 6 to 7. Conditions above 50°C and strong natural light are not conducive to the preservation and use of the extracts;
  • a bamboo leaf flavonoid beverage characterized in that it includes the following components by weight: moso bamboo leaf flavonoid extraction with a mass fraction of more than 50% 10 to 20 parts of liquid , 20 to 40 parts of bis-depleted apple juice, 3 to 5 parts of lemon juice concentrate, and 40 to 60 parts of water; the moso bamboo leaf flavonoid extract also contains moso bamboo leaf polysaccharide with a mass fraction of 5% to 7% ;
  • the present invention studies a high-energy beverage made by synergistically refining ultra-high-purity octacosanol-flavonoid compound deuterated water combination and its preparation method, which has strong application value.
  • bamboo leaf flavonoids or octacosanol alone in beverage processing technology.
  • the excellent properties of bamboo leaf flavonoids or octacosanol themselves are self-evident, and their combined use
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 98% extracted from fresh sugarcane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 95%;
  • the detritiated water has a deuterium content of 50 to 100 ppm.
  • the compound emulsifier is two or more of Tween 60, Tween 80, molecularly distilled monoglyceride, sucrose fatty acid ester, glyceryl monostearate, Span 60, and Span 80. A mixture of more than one species.
  • the stabilizer is one or a mixture of two or more of gum arabic, fish gelatin, xanthan gum, pectin, sodium carboxymethyl cellulose, cyclodextrin and konjac gum.
  • the compound electrolyte is a mixture of 0.65 parts of sodium citrate + 0.6 parts of calcium lactate + 0.37 parts of potassium chloride + 0.35 parts of magnesium lactate.
  • the water-soluble dietary fiber is one or two of modified polydextrose, partially hydrolyzed guar gum (PHGG), wheat starch resistant dextrin, corn starch resistant dextrin, and fructooligosaccharides. mixture.
  • modified polydextrose partially hydrolyzed guar gum (PHGG)
  • PHGG partially hydrolyzed guar gum
  • wheat starch resistant dextrin wheat starch resistant dextrin
  • corn starch resistant dextrin corn starch resistant dextrin
  • fructooligosaccharides mixture.
  • the sour agent is one or a mixture of two of citric acid, malic acid, lactic acid and bird's nest acid.
  • the preservative is one or a mixture of two of hydroxybenzoates, potassium sorbate, and nisin.
  • the high-energy beverage made by synergistically refining the combination of ultra-high purity octacosanol-flavonoid composite deuterated water and its preparation method includes the following steps:
  • the ultra-high-purity octacosanol-flavonoid compound deuterated water combination is a high-energy beverage that is synergistically refined. According to actual needs, by adjusting the changes in components, it is suitable for use in health care, beauty, weight loss, New generation sports drinks, astronauts, divers and military military high-energy drinks and other fields.
  • the high-energy drink made by synergistically refining the ultra-high-purity octacosanol-flavonoid complex deuterated water combination:
  • magic water also called high-energy drink
  • the original sports drink was a drink made by adding corresponding ingredients to the drink to replenish the water, sugar, salt, protein and vitamins that the human body loses during high-intensity exercise. Obviously, this is a passive supplement formulation concept;
  • the present invention uses ultra-high purity octacosanol-flavonoid compound deuterated water combination to supplement some special nutrients and coordinate with refined high-energy drinks to regulate these organs in a state of extreme fatigue in a targeted manner:
  • the present invention adopts the company’s [a supercritical-microwave-assisted ultrafine homogenate negative pressure cavitation high pressure combination one-step preparation method to strengthen the extraction of total flavonoids from bamboo leaves (Patent application number: 202210302314.1)] and the purity is ⁇ 95 % of bamboo leaf flavonoids, the analysis results of the main nutrients show that it contains flavonoids, active polysaccharides, phenolic acid compounds, anthraquinone compounds, manganese, zinc, selenium and other trace elements.
  • Flavonoids have obvious physiological activities such as anti-ulcer, antispasmodic, antibacterial, anti-inflammatory, hypolipidemic, and analgesic effects; active polysaccharides are sugar chains bonded by glycosylated bonds, which are beneficial to the human body's esophagus, bladder, kidneys, lungs, It has curative effects on liver and uterine cancer, and can promote wound healing, lower blood pressure, detoxify, and relieve fatigue.
  • the main mechanism is to enhance the body's liquid immunity and increase the activity of white blood cells and phagocytes; phenolic acid compounds can sterilize and make the body smell fragrant. It can refresh the brain, whiten the skin, clear away heat, relieve fire, nourish yin and nourish the skin. It can refresh the mind and reduce fatigue.
  • Anthraquinone compounds have hemostatic, antibacterial, purgative and diuretic effects. Trace elements are one of the six indispensable nutrients for the human body. It has various health-care effects such as clearing fire and improving eyesight, moistening the lungs and relieving cough, laxative and detoxification, soothing alcohol and soothing the nerves, promoting cell metabolism, improving blood circulation, and enhancing human immunity. It can also treat bronchitis, hypertension, hyperlipidemia, diabetes, etc. Diseases are cured well;
  • the dosage group of bamboo leaf flavonoids with a purity of 50% in the conventional market and the dosage group of bamboo leaf flavonoids with a purity of ⁇ 95% are used in the present invention.
  • the bamboo leaf flavonoids are melted with 1% gum arabic to prepare a corresponding dosage suspension, which is administered orally every day. once. Observe 5d. They were randomly divided into 2 groups according to body weight and weighed once a week. After 2 weeks, blood was collected from the eyeballs of rats without fasting to measure serum HDL-C;
  • the present invention uses the method described in our company’s [A preparation method for extracting octacosanol using an ultrasonic-microwave-assisted composite solvent secondary recrystallization and distillation synergistic refining combination (patent application number: 202210303916.9)] from fresh sugarcane filter mud.
  • Octacosanol with a purity of ⁇ 98% is extracted from it. It is a functional substance with anti-fatigue physiological activity. It has various physiological effects such as anti-fatigue, enhancing endurance and physical strength, improving myocardial function, and lowering blood lipids. It is a A very good natural health functional factor:
  • 3It can increase blood sugar and serum testosterone levels in bodies due to exercise fatigue and prevent myocardial damage
  • Reduces excess calcium and fat content in blood is a promoter of calcitonin formation, and can be used to prevent and treat hypercalcemia, osteoporosis, high cholesterol and high lipoprotein blood type diseases;
  • rats were randomly divided into 3 groups: the tail suspension group (hereinafter referred to as group A), the tail suspension plus octacosanol with a purity of 80% in the conventional market (hereinafter referred to as group B), and the tail suspension plus the octacosanol used in the present invention.
  • group A the tail suspension group
  • group B the tail suspension plus octacosanol with a purity of 80% in the conventional market
  • group B the tail suspension plus the octacosanol used in the present invention.
  • the octacosanol group with a purity of ⁇ 98% (hereinafter referred to as group C); 8 rats in each group, the supply amount is 25 mg/kg body weight per rat per day, the experimental period is 14 days; on the end of the experiment, the rats are fasted for 12 hours Afterwards, blood and tissue samples were collected; heart blood was collected by cardiac puncture, trunk blood was collected after decapitation, the thymus and spleen were removed and weighed, and the left hind limb femur was separated and removed; the weight of immune organs and the fluidity of red blood cell membranes were observed. and biomechanical properties of femur, etc.:
  • the weight of the thymus and spleen of rats in group B was significantly lower than that of rats in group A, but the weight of the thymus of rats in group C was 0.37g, which was significantly higher than that of rats in group B, 0.24g;
  • the thymus and spleen are important immune organs of the body, which suggests that the purity used in the present invention is ⁇ 98%.
  • the octacosanol has a certain protective effect on the decline of immune function caused by suspension simulated weightlessness;
  • the fluidity of the red blood cell membrane is usually expressed by the P value of the fluorescence polarization degree of the red blood cell membrane.
  • the larger the P value the smaller the hydrocarbon chain activity, the smaller the membrane fluidity, and the greater the blood microviscosity; conversely, the greater the membrane fluidity.
  • the larger the blood the smaller the microviscosity of the blood.
  • the average P values of the red blood cell membranes of rats in groups B and C were 0.28 and 0.32 respectively, which were significantly higher than 0.26 in rats in group A.
  • the viscosity of the blood of rats in group C was greater than that in group B. There is a downward trend compared with rats;
  • Table 2 shows the biomechanical measurement values of the femur obtained through the three-point bending test. After 14 days of tail hanging, the maximum load and elastic limit load of the femur of rats in group C were significantly higher than those in groups A and B. The results show that the octacosanol used in the present invention with a purity of ⁇ 98% can significantly resist the decline in the biomechanical properties of the femur of suspended rats;
  • Table 3 shows the biomechanical performance data of the femur calculated from the biomechanical and geometric parameters of the femur. The results show that the octacosanol group with a purity of ⁇ 98% used in the present invention can significantly improve the biomechanics of the suspended rat femur. performance;
  • the experiments show that the octacosanol used in the present invention with a purity of ⁇ 98% has the following functions on tail-suspended rats: 1 significantly increase the weight of the thymus; 2 improve the fluidity of the red blood cell membrane of simulated weightless rats; 3 significantly improve Femoral biomechanical properties; the octacosanol used in the present invention with a purity of ⁇ 98% can effectively combat certain adverse effects of tail-suspended rats; during the entire experimental process, no side effects of octacosanol were observed; It shows that a series of physiological and biochemical changes that occur in the body of astronauts under the condition of weightlessness can be used to improve exercise endurance by taking health drinks or foods added with octacosanol with a purity of ⁇ 98% used in the present invention. , reduce blood lipids, improve blood viscosity, improve hypoxic endurance and prevent osteoporosis, and may become a health drink or food ingredient for astronauts.
  • the deuterated water used in the present invention has a deuterium content of 25 to 100 ppm, and is used in disease prevention and drinking water.
  • the deuterium content is 1/7000 of hydrogen.
  • the deuterium content in natural water is generally 145-150ppm
  • the deuterium content in seawater is 155ppm
  • the deuterium content in glacier water is about 138-140ppm.
  • deuterated water is water that uses modern technology to reduce deuterium to 10-130ppm;
  • Deuterium has an accumulative effect in the body and is difficult to metabolize on its own. It can cause many adverse effects on the human body's DNA, heredity, metabolism and enzyme system;
  • deuterated water can be adapted to be used as an auxiliary product for other tumors such as prostate cancer, breast cancer, lung cancer, and pancreatic cancer;
  • deuterated water may provide new prevention strategies for depression
  • drinking deuterated water is also an option that can help achieve results.
  • deuterated water to make non-alcoholic beverages, such as drinking water, mineralized water, magnetized water, soft drinks and functional drinks, can improve human health and quality of life.
  • non-alcoholic beverages such as drinking water, mineralized water, magnetized water, soft drinks and functional drinks.
  • deuterated water products At present, the United States, Russia, Hungary, Ukraine, Japan, Germany, France, etc. have deuterated water products on the market. Low-deuterium water has been used in various metabolic diseases and cancers;
  • Deuterated water is not only used in scientific research. Deuterated water can activate immune cells, improve the body's basal metabolic level, resist cell mutation and delay Functions such as aging are more beneficial to the survival, development and reproduction of living organisms, and are of great significance to human health.
  • This invention uses water-soluble dietary fiber, an alternative and innovative solution for reducing sugar and replacing sugar.
  • This invention uses water-soluble dietary fiber technology to replace sugar.
  • the water-soluble dietary fiber used in the present invention is not only a high-quality water-soluble dietary fiber, but also a unique low-calorie filler; sugar is replaced with dietary fiber to reduce carbohydrate content and calories, and the plant-based one-to-one applied Sugar substitute; not only is it a good source of natural fiber, but it does not use any masking agents and has no aftertaste, giving it the same flavor as regular sugar;
  • Water absorption and expansion can increase the volume of feces, promote intestinal peristalsis, and have a good preventive effect on constipation, hemorrhoids, colon cancer and other diseases;
  • Resistant dextrin is recognized by the US FDA as a GRAS substance and has no intake limit.
  • resistant dextrin is widely used as a nutritional fortifier and has been recognized as a government-specified health food material by the Japanese Ministry of Health, Labor and Welfare.
  • the Ministry of Health [2012] Letter No. 516 plans to announce that resistant dextrin is a common food and can be added to various foods in unlimited amounts;
  • modified polydextrose is considered an important source of dietary fiber. Research shows that when young women drink a bottle of beverage containing 7-10g of modified polydextrose every day for 5 consecutive days, their feces will become significantly softer and constipation will be effectively relieved;
  • modified polydextrose is regarded as an important water-soluble dietary fiber
  • Fructooligosaccharides are fermented by bacteria in the large intestine to generate L-lactic acid, which can dissolve calcium, magnesium, iron and other minerals and promote the body's absorption of minerals. It inhibits the growth of harmful bacteria and regulates the balance in the intestine; it can promote the absorption and utilization of trace elements iron and calcium to prevent osteoporosis; it can reduce liver toxins and generate anti-cancer organic acids in the intestine, which has significant anti-cancer effects.
  • fructooligosaccharide promotes calcium absorption by 70.8%. Therefore, fructooligosaccharides can promote growth and development and prevent osteoporosis; at the same time, it can also promote the natural formation of vitamins B1, B2, B3, B6, B12 and folic acid, thereby improving the body's metabolism, immunity and disease resistance. Prevent and improve skin diseases caused by toxins in the body, prevent facial sores, dark spots, freckles, acne, and age spots, make the skin bright and slow down aging.
  • Bifidobacterium absorbs fructooligosaccharides, it rapidly proliferates, inhibits the action of spoilage bacteria such as Escherichia coli, Salmonella and Clostridium, reduces the production of toxic metabolites (such as indole, nitrosamine), and rapidly metabolizes the toxicity oligosaccharides are excreted from the body, reduce the burden on the liver, protect the liver, and prevent various chronic diseases, cancers, etc.; fructo-oligosaccharides are rarely decomposed by gastric acid and enzymes in the digestive tract, and are extremely difficult to be absorbed by the human body;
  • the caloric value of fructo-oligosaccharide is less than 1.5Kcal/g, while the caloric value of sucrose is 4.6Kcal/g. Therefore, after ingesting fructo-oligosaccharide, it will not cause obesity and is an ideal low-calorie functional sweetener. .
  • Fructooligosaccharides cannot be used by Streptococcus mutans to generate insoluble glucan and provide a place for oral microbial deposition, acid production and corrosion (tartar), thus preventing dental caries.
  • the present invention has discovered and verified through experimental research: The influence of various factors on the stability of a high-energy beverage collaboratively refined with an ultra-high-purity octacosanol-flavonoid compound deuterium-free water combination:
  • emulsifier type and dosage plays an important role in the formation of a stable emulsion system; a suitable emulsifier can significantly reduce the surface tension between the two phases, change the interface state of the system, and help stabilize the uniform dispersion of droplets. ;
  • the oil-soluble emulsifier Span 80 was selected as an example to conduct experiments to examine the stabilizing effect of its dosage on beverages;
  • Tween 80 was selected as an example to conduct experiments to examine the stabilizing effect of its dosage on beverages;
  • This experiment selected three commonly used hydrophilic colloids: xanthan gum, sodium carboxymethyl cellulose (CMC), and gum arabic as stabilizers to conduct a single-factor test on body stability. Under the same conditions, the beverage was observed to change from static to static. When a large amount of precipitation occurs, the type of stabilizer required for the final test will be determined based on the stabilizing effect;
  • xanthan gum sodium carboxymethyl cellulose (CMC), and gum arabic have better effects when used alone in beverages.
  • CMC carboxymethyl cellulose
  • xanthan gum has the best effect, which is in line with its own growth rate. Characteristics of the strongest thickening effect;
  • Xanthan gum serves as a thickener, emulsifier, and stabilizer. Due to its pseudoplasticity, xanthan gum can increase the richness of the drink and stabilize the suspension of each component. It is thickened but not sticky, and has good fragrance release; As an emulsification aid in beverages, gum arabic has good water solubility and emulsification as a food adhesive. During the embedding process, it can increase the efficiency of the embedding, enhance the taste, prevent precipitation and maintain the flavor of the capsule; carboxyl Sodium methylcellulose (CMC) has multiple functions such as thickening, suspension, emulsification, and stabilization. It has good water retention, dispersion, and thixotropy, and can control the size and growth of ice crystals during transportation and storage. Used as a protective agent for beverages; therefore, the combination of the above three can prevent beverages from agglomerating;
  • 1.8x104r/min is selected as the optimal emulsification speed; the emulsification time is too short, the emulsification process is not sufficient, and the floating phenomenon of the drink is serious; when the emulsification process is basically completed, extending the stirring time will have minimal improvement in stability. , has little value in actual production, so the emulsification time is 25 minutes;
  • Homogenization is a common physical method to prevent precipitation and stratification of beverages.
  • the choice of homogenization temperature and pressure directly affects the homogenization effect.
  • the pressure is 30-35Mpa and the temperature is 60-70°C to homogenize the beverage.
  • the test shows that when the pressure is 30-35Mpa and the temperature is 60-70°C, there is no stratification of the product when homogenized twice. , floating and settling phenomena. It can also be seen from the experiment that the greater the pressure, the higher the temperature, the more times of homogenization, and the finer the particles, but the temperature and pressure are too high. Too many times of homogenization will consume too much production cost.
  • the pressure is 30-35Mpa
  • the temperature is 60-70°C
  • the homogenization is performed twice.
  • the first homogenization is 3 to 4 minutes with an interval of 25 minutes;
  • the second homogenization is 1 to 2 minutes.
  • the diameter is 3 ⁇ m. ⁇ 5 ⁇ m oil-in-water droplets. It can produce drinks with good quality, good texture and stable structure;
  • high shear emulsification time > water-soluble emulsifier dosage > oil-soluble emulsifier dosage > stabilizer dosage;
  • UHT 105-121°C, 6-10 seconds
  • the purity of flavonoids and octacosanol must reach at least 90% to achieve the effects of effectively lowering lipids and preventing cardiovascular and other diseases.
  • the purity used in the present invention is ⁇ 95% bamboo leaf flavonoids and octacosanol with a purity of ⁇ 98% can be used in beverages not only for anti-fatigue and improving human body function, but also for further development in fields such as disease prevention;
  • the present invention proposes a synergistic combination of ultra-high-purity octacosanol-flavonoid complex deuterium-free water, which can be reasonably and effectively strengthened and improved by cross-comparison and integration based on the characteristics of each extract. It regulates complementary and synergistic effects, which is beneficial to absorption and circulation in the body; it introduces ultra-high purity extracts into beverages, changing the concept of passive supplementation and creating the concept of actively conditioning beverages.
  • the present invention solves the problem of poor water solubility of octacosanol and flavonoids. It will not cause any flavor and sensory problems in the beverage and has good uniformity;
  • the materials selected are made from halal certified raw materials, without religious distinction; sugar-free, pigment-free, green, pure and healthy, which also provides quality and safety guarantee for halal high-energy drinks;
  • Figure 1 shows the purity test report of bamboo leaf flavonoids extracted from this product.
  • Figure 2 shows the results of the purity test report of bamboo leaf flavonoids extracted from this product.
  • Figure 3 is the purity test report of octacosanol extracted from fresh sugarcane filter mud by this product.
  • Figure 4 shows the purity test report results of this product extracting octacosanol from fresh sugarcane filter mud.
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 98% extracted from fresh sugarcane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 95%;
  • the deuterated water has a deuterium content of 25 to 100 ppm.
  • Its preparation method includes the following steps:
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 98% extracted from fresh sugarcane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 95%;
  • the deuterated water has a deuterium content of 25 to 100 ppm.
  • Its preparation method includes the following steps:
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 98% extracted from fresh sugarcane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 95%;
  • the deuterated water has a deuterium content of 25 to 100 ppm.
  • Its preparation method includes the following steps:
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 98% extracted from fresh sugarcane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 20%;
  • the deuterated water has a deuterium content of 25 to 100 ppm.
  • Its preparation method includes the following steps:
  • An ultra-high-purity octacosanol-flavonoid composite deuterated water combination synergistically refined high-energy drink and its preparation method including the following components: 0.05 to 0.1 parts of octacosanol, 0.12 to 0.2 parts of flavonoids, and deuterated water. 900 to 1000 parts of water, 0.1 to 0.3 parts of stabilizer, 0.3 parts of compound emulsifier, 15 to 25 parts of water-soluble dietary fiber, 1.97 parts of compound electrolytes, 0.03 to 0.6 parts of preservatives, and 0.05 to 0.2 parts of sour agent;
  • the octacosanol is octacosanol with a purity of ⁇ 80% extracted from fresh sugar cane filter mud;
  • the flavonoids are bamboo leaf flavonoids with a purity of ⁇ 95%;
  • the deuterated water has a deuterium content of 25 to 100 ppm.
  • Its preparation method includes the following steps:
  • Example 1 In order to observe the effect of high-energy drinks on the concentration of serum high-density lipoprotein cholesterol in rats, a comparative experiment was carried out between Example 1 and Control Example 1-1, and the serum high-density lipoprotein cholesterol (HDL-C) level index of rats was measured. , giving specific data reference for the effect of high-energy drinks on increasing density lipoprotein cholesterol (HDL-C):
  • Rats were selected, provided with basic feed, and had free access to water and food; the room temperature in the breeding room was 23 ⁇ 5°C, the relative humidity was 40% to 70%, and the lighting changed naturally. After the animals were observed and adapted for 5 days, 80 animals were selected for experiments and randomly divided into 4 groups. Three of the groups were fed mixed high-fat animal model feed: 20% sucrose, 15% lard, 1.2% cholesterol, 0.2% sodium cholate, 6.6% casein, 0.5% calcium hydrogen phosphate, 0.3% stone powder, and the drinking water of two of the three groups of mice was replaced with the high-energy drink prepared in Example 1 and Comparative Example 1-1. of high-energy drinks. Weigh once a week, record food intake and calculate food utilization. The trial lasts for 30 days.
  • the bamboo leaf flavonoids used in the present invention have a purity of ⁇ 95%, the serum HDL-C concentration of the test rats can be significantly increased.
  • the bamboo leaf flavonoids with a purity of 20% are used, the serum HDL-C concentration is not significantly increased ( Table 10).
  • Example 1 In order to observe the effects of different purity extracts of high-energy drinks on improving the swimming time and anti-fatigue effects of mice, a comparative experiment was carried out between Example 1 and Control Examples 1-2. 30 rats were taken and randomly divided into Example 1 Prepare beverages (hereinafter referred to as beverage group A), prepare beverages in Comparative Examples 1-2 (hereinafter referred to as beverage group B), deionized water blank control group (hereinafter referred to as group C), 10 mice in each group, and administer intragastric administration to mice , 10ml each, the dosage is equivalent to 3g/kg, administered continuously for 15 days and 30min after the last dose:
  • mice were placed on the upper end of a vertically suspended smooth glass rod, so that their muscles were in a state of static tension. The mice were recorded from climbing the rod until their muscles were fatigued and unable to hold the glass rod and fell to the ground. Time, repeat 3 times, terminate the test after the third fall, and the cumulative time of 3 times is used as the pole climbing time (s);
  • mice Each group continued to be administered intragastrically for 5 days. 30 minutes after the last administration, 8% of the body weight was weighted with a lead wire at the base of its tail. The mice were placed in a swimming box at room temperature, and the time from the beginning of swimming to the death of the mice was recorded. swimming time (min);
  • Deionized water blank control group experiment Mice were given deionized water by gavage, 10 ml each, at a dose equivalent to 3g/kg, for 5 consecutive days, and then performed weight-bearing swimming 30 minutes after the last administration, in room temperature water. Put 8% of the body weight on the tail with a lead skin, swim until exhaustion, sink into the water and stay up for 10 seconds, record the time;
  • mice in each group were administered intragastrically for 5 days. 30 minutes after the last administration, they were put into normal temperature water for 60 minutes and then taken out. Blood was taken from the supraorbital venous plexus and serum urea nitrogen was measured using a kit method. Then the animals were killed immediately, the liver was removed, rinsed with 0.9% NaCl solution, dried with filter paper, and the liver glycogen content was measured by the anthrone method;
  • mice After mice were gavaged for 15 days and swam under weight, the blood lactate in group A was significantly lower than that in group B, indicating that this effect may be related to the purity of the test substance;
  • liver glycogen content of group A was significantly higher than that of group B, indicating that the octacosanol used in the present invention with a purity of ⁇ 98% can improve the glycogen accumulation capacity in animals;
  • the serum urea nitrogen level was measured after swimming in mice administered intragastric administration for 20 days.
  • the level of serum urea nitrogen in group A was significantly lower than that in group B.
  • the difference was extremely significant, indicating that the octacosanol used in the present invention with a purity of ⁇ 98% can significantly reduce the serum urea nitrogen level.
  • Urea nitrogen improves the body's endurance and adaptability to exercise load;
  • beverage group A uses octacosanol with a purity of ⁇ 98%, it has a significant anti-fatigue effect, indicating that the high-energy beverage of the present invention has an anti-fatigue health care effect;
  • beverage group B uses It is low-purity octacosanol, and its anti-fatigue effect is significantly lower than that of beverage group A.
  • a method for preparing bamboo leaf flavonoid extract through column purification 200910223926.6 shows that the purity of bamboo leaf flavonoids is 20.78%;
  • a production method for extracting bamboo leaf flavonoids from bamboo leaves 200610053134.5 shows that the purity of bamboo leaf flavonoids is ⁇ 24%;
  • a method for separating and purifying flavonoids and lactones from bamboo leaves based on microwave-assisted technology CN201510481490 shows that the purity of bamboo leaf flavonoids is ⁇ 29%;
  • a preparation method of bamboo leaf flavonoids extract 200910223927.0 shows that the purity of bamboo leaf flavonoids is 42%;
  • a method for extracting flavonoids from bamboo leaves 201110003352.9 shows that the purity of bamboo leaf flavonoids is 30 ⁇ 50%;
  • a method for extracting bamboo leaf flavonoids 201110406495.4 shows that the purity of bamboo leaf flavonoids is 30 ⁇ 50%;
  • the production process for extracting bamboo leaf flavonoid series products from bamboo leaves 200610053436.2 shows that the purity of bamboo leaf flavonoids is 60%;
  • bamboo leaf flavonoids extract 200810195064.6 shows that the purity of bamboo leaf flavonoids is 40%-65%;
  • Zhu Hongli et al. extracted the crude bamboo leaf extract with chloroform, and then passed the chloroform layer sample through X-5 macroporous resin. After elution with a high-concentration alcohol solution, the primary purified sample was passed through a polyamide column. The total flavonoid content in the purified sample can reach 78.97%;
  • the article shows that the flavonoid content of the obtained bamboo leaves reaches more than 40%
  • the bamboo leaf flavonoids described in Reference Document 2 are only a conceptual summary, and are actually just a crude extract with low extraction rate and many impurities (such as phenols, Saponics, whiplash, alkaloids, polysaccharides, protein, crude fat, chlorophyll, anthraquinone compounds, mushroom lactosides, inorganic salts, moisture, minerals, ash, heavy metals, arsenic and manganese, zinc , selenium and other trace elements, more than 20 mineral elements, 82 aromatic compounds, 16 amino acids, 53 volatile components, 10 alcohols, 17 aldehydes, etc.), the so-called bamboo leaf flavonoids are only the components of these substances Some of the contents are, at best, just a trade name.
  • Zhang Xiangnian et al. melted the insect wax, poured it into ether, and used the reduction method to catalyze it with LiAIH4. After reduction at 70-80°C for 2.5 hours, a high-carbon fatty alcohol mixture was obtained. After purification by molecular distillation, a mixture containing 16.7% octacosanol was obtained. Small quantity of product.
  • Wang Xingguo et al. used crude bran wax as raw material, refined it, and used ultrasonic hydrolysis of rice bran wax, extraction of fatty alcohols, and molecular distillation technology to separate octacosanol and triacontanol to prepare products with a purity greater than 80%.
  • Xiamen University Chemical Plant uses Sichuan and other beeswax as raw materials, and uses the residue from the production of triacontanol to extract octacosanol.
  • the purity is 12.8% and 18%.
  • Xiamen University also uses insecticide wax as raw material to produce octacosanol.
  • the outstanding disadvantage is that the cost is high, and the content of octacosanol has not made a big breakthrough.
  • Wheat germ beverage and its preparation method - 201010615889.6 The octacosanol described in claim 4 is first extracted from the wheat germ using a supercritical CO2 extraction method to obtain white flake crystals of octacosanol, of which 28 Alkanol content is 42.1 ⁇ 43.5%;
  • the 24-34 carbon higher alkanols contained in Cuban Policosanol account for more than 90% of the weight of the extract, of which the octacosanol content is 60%-70%.
  • octacosanol In Japan, most octacosanol is extracted from rice bran oil and rice germ oil. The content of octacosanol is generally 10% ⁇ 15%, which is a mixture of C22 ⁇ C36 fatty alcohols. Most of the octacosanol produced by octacosanol is made from rice bran oil and rice germ oil. The octacosanol content in octacosanol products is usually 12%.
  • octacosanol purified by most international and domestic manufacturers is generally about 12%, which is a mixture of C22 ⁇ C36 fatty alcohols. Even Japanese octacosanol products only contain about 15%.
  • the early products of octacosanol were mainly wheat germ oil concentrates; currently, except for Japan’s progress in using rice bran to produce octacosanol, there is no large-scale production technology of octacosanol from rice bran abroad. No advantage.
  • the current main raw materials for extracting octacosanol are rice bran wax, wormwood, wheat germ oil, and sugar cane wax, because it is insoluble in water and soluble in organic solvents, and the structure of the existing substance is relatively complex, currently such substances are If the raw material is saponified and extracted with an organic solvent (n-hexane, acetone, etc.), a white or light yellow powdery body will be obtained.
  • This powdery crystal is a natural high-grade alkanol mixture (containing 24-34 carbon atoms). Higher alkanols), the current product technology only contains less than 50% octadecane.
  • the conventional extraction purity of octacosanol can only reach 15-35%.
  • the bamboo leaf flavonoids described in Reference Document 2 are only a conceptual summary, and are actually just a crude extract with low extraction rate and many impurities (such as phenols, Saponics, whiplash, alkaloids, polysaccharides, protein, crude fat, chlorophyll, anthraquinone compounds, mushroom lactosides, inorganic salts, moisture, minerals, ash, heavy metals, arsenic and manganese, zinc , selenium and other trace elements, more than 20 mineral elements, 82 aromatic compounds, 16 amino acids, 53 volatile components, 10 alcohols, 17 aldehydes, etc.), the so-called bamboo leaf flavonoids are only the components of these substances Some of the contents are, at best, just a trade name.
  • bamboo leaf flavonoids and octacosanol of different purity have different effects in different fields. Because the higher the purity of bamboo leaf flavonoids and octacosanol, the stronger their activity and greater polarity. If you want to effectively lower lipids, prevent cardiovascular and other diseases, improve hypoxic endurance and prevent osteoporosis, For performance and other effects, the purity must reach at least 90%. Therefore, purity determines the physiological activity of a drug;
  • the octacosanol used in the present invention is extracted from fresh sugar cane filter mud with a purity of ⁇ 98%; the flavonoids used are bamboo leaf flavonoids with a purity of ⁇ 95%. According to the characteristics of each extract, crossover and integration are carried out, and ultra-high purity extracts are introduced into beverages, which changes the concept of passive supplementation and creates the concept of actively conditioning beverages, which reasonably and effectively greatly strengthens and improves the complementary and synergistic effects of beverages on body regulation.

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Abstract

一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇、黄酮、去氘水、稳定剂、复配乳化剂、水溶性膳食纤维、复配电解质、防腐剂、酸味剂;所述二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇,所述黄酮为纯度≥95%的竹叶黄酮,所述去氘水的氘含量为25~100ppm。

Description

一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法 技术领域
本发明涉及食品加工技术领域,具体设计一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法。
背景技术
⒈二十八烷醇是一种天然的高级脂肪醇,具有良好的生物降解性,易于被人体吸收
⑴从1949年开始,美国依利诺斯大学的T.K.Cureton博士等花费了20年的时间,进行了894名受试人员经42项目的测试研究,参加实验的人员有游泳、摔跤、田径等队员,体育专科学生、美国海军、海军潜水员等。归纳这些实验结果,二十八烷醇具有新陈代谢比率、降低肌肉摩擦,从而达到减少必要的需氧量、改进反应时间、消除肌肉疼痛等功效,并且这些作用是相互关联的;确定了二十八烷醇积极促进人体生理功能的主要功效为:
①增强耐力,精力和体力;
②提高肌肉力量(肌肉机能);消除肌肉疼痛,减少肌肉摩擦;
③缩短肌神经反应时间,提高应激能力;提高反应敏锐性;
④强化心脏机能,改善心肌功能;
⑤提高应激能力、机体新陈代谢的比率;
⑥增强对高山等应力的抵抗性;
⑦降低收缩期血压;
⑧提高氧的输送能、机体氧利用率,减少必要的需氧量;
⑨刺激性激素;
⑩降低胆固醇;
⑵“三高”是威胁现代人类健康的一类发病率较高的病症
早在2006年,钟耕等人已经证实二十八烷醇具有降低血脂的功能。祁晓鸣等人提出,二十八烷醇的降血脂功效与用量有关,较高用量的该物质可以显著减小血清中的TG、TC以及LDL-C心含量;而低剂量的仅对血清里的TC浓度有影响。DevK.Singh等人的研究提出,二十八烷醇降低血清中的胆固醇含量,是通过AMP-激酶的磷酸化来激活酶活性,从而减小HMG -CoA酶活性,达到控制血清中胆固醇合成的目的;
⑶二十八烷醇能减少血液过多钙质和脂肪含量、是降血钙素形成促进剂
可用于治疗血钙过多骨质疏松症,高胆固醇和高脂蛋白血型疾病,可用于治疗老年初期帕金森氏病。经过多方证实,二十八烷醇被誉为是能够缓解身体疲劳并具有良好生物活性的一种化合物。研究表明,该物质能够提升人体的耐力、快速恢复体力,以及改善活动后的体液内的相关生理指标等动能;
⑷可提高运动性疲劳大鼠的血糖、血清睾酮水平,防止心肌损伤,对人体的生殖障碍;可提高机体的耐缺氧能力,疾病有治疗作用,研究发现二十八烷醇减轻心脑组织血管轻度扩张、细胞水肿,对组织细胞的结构有一定保护作用,还具有潜在的抗炎、抗肿瘤功效;
⑸二十八烷醇的一个显著特点是用量极微而生理活性显著,能够快速消除疲劳,增强体力和耐力,为世界公认的抗疲劳功能性物质。根据日本油脂株式会社的报道,通常每人每天口服0.2mg的二十八烷醇就能达到消除疲劳的目的;为了增强体力和耐力,每天的口服量大约是0.5mg;而用于治疗目的的用量为5mg;
⑹其安全性极高。经小白鼠口服试验证明,二十八烷醇的 LD 50 为18000mg/kg以上;安全性比食盐 (LD 50=3000mg/kg)还高得多;经临床实践证明,可长期服用而无副作用。
⒉竹叶黄酮属于植物黄酮的一种,有效成分是黄酮糖苷和香豆素类内酯。其成分除了黄酮类化合物以外,还有酚酸、蒽醌类化合物、芳香成分和锰、锌、锡等微量元素,它们共同构成了竹叶黄酮广泛的生理和药理活性的基础
⑴一项由荷兰专家主持的研究发现:由 4807位参与者的实验表明,每天饮 375毫升绿茶的人,其心脏病的发病概率是那些不喝茶的人的一半;致命性心脏病发病率只有三分之一。其中重要的原因就是绿茶中所含的黄酮(<<美国临床营养学>>2002.4.25) ;
对竹叶黄酮的生理功效进行了调查研究表明:
①具有清除氧自由基、抗衰老、预防老年性痴呆、防止血管硬化、抗血管增生、抗心肌缺血、降血压、降血脂、保护心脑血管,用于防治心脑血管疾病,如能降低血管的脆性,舒张血管和改善血管的通透性、防止动脉硬化、降低血脂和胆固醇,防治老年高血压、脑溢血、冠心病、心绞痛、扩张冠状血管,增加冠脉流量、降低血糖等方面均具有良好的效果;
②能够诱发癌细胞和肿瘤细胞的凋亡,发挥抗癌抗肿瘤作用,而对正常组织细胞的凋亡起延缓作用;
③防辐射、保肝、解肝毒、治疗急、慢性肝炎、肝硬化、提高机体免疫力、泻下、止咳、祛痰、平喘、解痉及抗***、抗变应性和抗病毒等药理功效;
⑷几乎所有类黄酮对很多微生物(包括革兰氏阳性菌、革兰氏阴性菌和真菌),都具有程度不等的抑菌活性;
⑤可提高机体免疫机能,促进机体健康; 
⑥不仅有较多药用功效,还具有较好稳定性,因结构中含酚羟基,与人体胃液、肠液酸性环境一致,可避免首关效应;
   具有以下几个方面的突出优点: 
①结构稳定,不易被降解; 
②能深入病灶部位,直接发挥疗效;
 ③亲水性增强,有利于药品、食品、化妆品等的开发;
⑵抗疲劳
氧化应激被证明通过增加释放促炎细胞因子,如肿瘤坏死因子-α(TNF-α)、白细胞介素-6(IL-6)和IL-1β导致慢性疲劳;  
许多研究表明,补充黄酮类化合物可减轻疲劳大鼠肌肉疲劳。在对黄酮类化合物的研究中,从毛竹中分离得到的叶黄素-6-c-新橙皮苷木犀草素-6-C-新橙皮糖苷(LN),在小鼠负重试验强迫游泳实验中 LN对小鼠有抗疲劳作用。经 3周大鼠游泳模型验证,LN可明显延长大鼠疲劳时间,从而实现抗疲劳效果;
⑶抗衰老的作用   
人类的疾病大概有70多种,包括癌症、心脑血管病都与自由基有关,竹叶黄酮能有效地清除自由基,产生抗氧化的作用,从而达到延缓衰老的目的;    
⑷减肥的功效   
人体营养过剩转化为脂肪,储存在体内的脂肪会氧化变性,这是肥胖者难以减肥的原因之一,生物黄酮有预防脂质过氧化作用,减少脂肪积存,成为新的减肥途径; 
⑸是一种天然抗氧化物
①可以明显降低运动后血乳酸的含量,同时增强乳酸脱氢酶的活力;
②抗氧化性能可以与VE相媲美,作为新型的抗氧化剂,竹叶黄酮可防止或延缓食品被氧化,提高食品的稳定性和延长贮存期;
⑹具有抑菌功能,可以应用于食品工业中;
⑺安全无毒
在其有效成分中,迄今尚未发现任何有毒、有害成分,不像银杏叶中含有一定量的白果酸,对人体有害;
关于竹叶的药效,在《本草求真》、《药品化义》等古籍和现在的《中药大辞典》中均有记载;
1998 年,(淡)竹叶又被***批准列入“药、食两用的天然植物名单。”可见竹叶本身就具有安全使用性;
近年来的研究报道表明:对竹叶黄酮釆用急性毒性试验(霍恩氏法) ,据Ames试验结果判断标准,所测试的竹叶黄酮无致突变作用;
并且浙江省医学科学院于 1998-1999年间又对竹叶黄酮粉、竹叶黄酮进行毒理学安全性评价,证实了竹叶黄酮无毒副作用,具有很高的安全性。
⒊开发现状、方向、重点
⑴二十八烷醇
由于目前二十八烷醇的主要提取原料为蔗赌、糠蜡、虫姑、小麦胚芽油,由于它不溶于水,溶于有机溶剂,加之存在物的结构比较复杂,因此,如何从天然物高效、经济、环保的提取,便是得到大量高品质此类物质在生产中应解决的问题,而目前这类物质上要是原料经皂化后用有机溶媒(正己烷、丙酮等)提取,得到一种白色或浅黄色粉末状品体,此粉末状晶体为天然髙级烷醇混介物(含有24-34个碳原了高级烷醇),此混合物中二十八烷含量为 50-70%,而资料中有关药理实验也是以此含量的提取物进行的。目前该产品技术也只是二十八烷醇的常规提取纯度只能达到40-80%,如:一种运动饮料及其制造方法-200510036559.0(无权-未缴年费)权利要求5.所述的运动饮料,其特征在于: 所用二十八烷醇的纯度大于80%。如:小麦胚芽饮料及其制备方法-201010615889.6(无权-未缴年费)权利
要求4.所述的二十八烷醇是先采用超临界CO2 萃取方法从小麦胚芽中萃取,获得二十八烷醇白色片状结晶, 其中二十八烷醇含量为42.1~43.5%
⑵传统黄酮的提取方法
黄酮类化合物因其结构和来源的不同 ,溶解特性差异也很大,因此,应据其极性和水溶性的大小选择合适的溶剂进行提取。随着研究的不断深入,对竹叶黄酮的提取方法也越来越多,根据文献,竹黄酮类化合物常见的提取方式有热水提取法、有机溶剂提取法、微波提取法、超声波提取法、超临界流体萃取法、酶提取法、破碎提取法等多种方法;
实验结果表明,微波提取竹叶黄酮效率最高,超声提取次之,水浸提效率最差,耗时长且提取率低,但是水浸提浸提所得的竹叶黄酮稳定性相对较好;
上述各种单一方法所得的提取液在 pH 为6~7范围内稳定性较好,高于50℃和强光自然光条件不利于提取液保存及使用;
上述各种单一方法对于黄酮的单次提取率不高,一般为40-60%,均需3次或以上多次,且即使3次或以上多次提取后纯度也只有30-50%;如:一种竹叶黄酮饮料及其制备方法202010982466 .15的权利要求1.一种竹叶黄酮饮料,其特征在于,其包括以下重量份的组分:质量分数为 50%以上的毛竹叶黄酮提取液10~20份、双脱苹果汁20~40份、柠檬浓缩汁3~5份、水40~60份;毛竹叶黄酮提取液中还包含有质量分数为5%~7%的毛竹叶多糖;
技术问题
综上所述,对二十八烷醇和竹叶黄酮的提取方法虽然已经有一定的成果,但:
①目前市场上述这种纯度只能用于抗疲劳和提高人体机能的保健作用,若想达到有效降脂、预防心血管等疾病的效果,纯度至少要达到90%,因而限制了其在食品及医药领域的进一步发展,因此,纯度决定一个药物的生理活性;而且也给进一步分离带来很多麻烦,后续精制工艺流程操作相对繁琐、费时;
②目前市场上进行单一添加二十八烷醇或竹叶黄酮的功能性饮料种类很多,但单一体系方式限制了应用范围和效果;在功能性饮料工业运用上还有一定的局限性。
⒋本发明研究一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,具有较强的应用价值
目前单独的竹叶黄酮或者二十八烷醇用在饮料加工技术中都有一定的在先技术尝试,而竹叶黄酮或者二十八烷醇本身的优良性质已经不言而喻,其组合运用的方式方法如今尚未见有较为成功的案例;一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,该方面尚未见报道。
解决方案
因此,提供一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,是符合人们期望的。
为了达到上述目的,本发明所采用的技术方案是:
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
所述的黄酮为纯度≥95%的竹叶黄酮;
所述的去氚水为氘含量50~100ppm。
优选的,所述的复配乳化剂为吐温60、吐温80、分子蒸馏单甘酯、蔗糖脂肪酸酯、单硬脂酸甘油酯、司盘60、司盘80中的两种或两种以上的混合物。
优选的,所述的稳定剂为***胶、鱼明胶、黄原胶、果胶、羧甲基纤维素钠、环状糊精、魔芋胶中的一种或两种以上的混合物。
优选的,所述的复配电解质为柠檬酸钠0.65份+乳酸钙0.6份+氯化钾0.37份+乳酸镁0.35份的混合物。
优选的,所述的水溶性膳食纤维为改性聚葡萄糖、部分水解瓜儿豆胶(PHGG)、小麦淀粉抗性糊精、玉米淀粉抗性糊精、低聚果糖中的一种或两种的混合物。
优选的,所述的酸味剂为柠檬酸、苹果酸、乳酸、燕窝酸中的一种或两种的混合物。
优选的,所述的防腐剂为羟基苯甲酸酯类、山梨酸钾、乳酸链球菌素中的一种或两种的混合物。
优选的,所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水900~1000份、水溶性膳食纤维15~25份加入密封反应釜内,开启搅拌,转速为300~500r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.05~0.1份、黄酮0.12~0.2份、稳定剂0.1-0.3份、复配乳化剂0.3份,同时加热至85℃,在1.8X104r/min的高剪切速度下乳化25min;降温至60-70℃,再利用均质机经压力30-35Mpa,均质两次,第一次均质3至4min,间隔25min;第二次均质1至2min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份加入步骤⑴中的基料,转速为300~500r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,6-10秒;
⑷灌装:得到一种二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
优选的,所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料,根据实际需要,通过调节组分的变化,适宜用作于保健、美容、减肥、新一代运动饮料、航天员、潜水员和军队军需高能饮品等领域。
优选的,所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料:
⑴选用的材料,不含哺乳类动物性成份,无疯牛症、***等人畜共通传染病隐忧,来源丰富,安全性高;
⑵为清真认证原料制成,无宗教区分。
有益效果
⒈首创采用超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料
现在世界上悄然兴起一种称之为“魔水”(又叫高能饮料)的运动饮料,就是在原运动饮料的基础上增加了中药成分,从而使其具有突出功效。最初的运动饮料是补充人体在高强度体育运动时大量流失的水份、糖份、盐、蛋白质和维生素等,有针对性的在饮料中添加相应的成分而制成的饮料。很显然,这是一种被动补充的配制理念;
    从现代医学理论来看,体育属于一种极限体力活动,在剧烈运动后,人体不仅仅是损失了上述大量的营养物质,而且一些器官因为超强的运动而产生一些功能的透支,处于极度疲劳状态,难以迅速复原,例如大脑、心脏、消化***以及免疫***。这时运动员会在夜间睡眠不好,心跳过速、食欲减退、胃肠吸收功能差、易感染疾病等;
    这些又反过来延迟人体机能的全面恢复,这种身体状态,就不是简单的补充水、盐等物质所能解决的;
本发明采用超高纯度二十八烷醇-黄酮复合去氘水组合,补充一些特殊的营养物质,协同精制的高能饮料,有针对性地对这些极度疲劳状态下的器官进行调节:
⑴本发明采用本公司【一种超临界-微波辅助超微细匀浆负压空化高压组合一步法强化提取竹叶总黄酮的制备方法(专利申请号:202210302314.1)】的所述纯度为≥95%的竹叶黄酮,主要营养成分分析结果显示:含有黄酮类化合物、活性多糖以及酚酸类化合物、蒽醌类化合物和锰、锌、硒等微量元素。黄酮类化合物有明显的抗溃疡、解痉、抗菌、抗炎、降血脂、镇痛等生理活性作用;活性多糖是由糖昔键结合的糖链,对人体的食道、膀胱、肾脏、肺、肝和子宫癌均有疗效,可促进创伤治愈、降血压、解毒、减轻疲劳,主要机理是增进人体液体性免疫,提高白血球吞噬细胞的活性;酚酸类化合物可以杀菌,还可以使体味芬芳,醒脑提神,美白肌肤,清热、解火滋阴养颜,可以提神,减少疲劳的功效;蒽醌类化合物具有止血、抗菌、泻下、利尿的作用;微量元素是人体不可缺少的六大营养素之一,具有清火明目、润肺止咳、通便解毒、解酒安神,促进细胞新陈代谢,改善血液循环,增强人体免疫力多种保健作用,并对气管炎、高血压、高血脂、糖尿病等多种疾病有良好疗效;
在功能饮料中体现为:
①是一种天然抗氧化物
可以明显降低运动后血乳酸的含量,同时增强乳酸脱氢酶的活力;
②抗衰老的作用   
人类的疾病大概有70多种,包括癌症、心脑血管病都与自由基有关,竹叶黄酮能有效地清除自由基,产生抗氧化的作用,从而达到延缓衰老的目的;    
③减肥的功效   
人体营养过剩转化为脂肪,储存在体内的脂肪会氧化变性,这是肥胖者难以减肥的原因之一,生物黄酮有预防脂质过氧化作用,减少脂肪积存,成为新的减肥途径; 
④其多功能性
除了高效的抗脂质氧化性外,还是一种天然的黄色素,兼具抗菌、抑菌、除臭、增香的作用;
本发明经实验研究发现并验证了竹叶黄酮纯度对大鼠血清高密度脂蛋白胆固醇浓度的影响:
常规市场纯度为50%的竹叶黄酮剂量组和本发明采用的纯度为≥95%竹叶黄酮剂量组,竹叶黄酮用1%***胶溶融制成相应剂量的悬浮液,每天经口灌胃一次。观察5d。按体重随机分成2组,每周称重1次。2周后,大鼠不禁食眼球采血,测定血清HDL-C;
表1   竹叶黄酮对大鼠血清HDL-C浓度的影响(平均值)
实验开始时,各组血清中HDL-C浓度无明显差异;在给药2周后,本发明采用的纯度为≥95%竹叶黄酮可显著提高试验大鼠血清HDL-C浓度,常规市场纯度为50%的竹叶黄酮提高血清HDL-C浓度不明显(表1),研究表明高纯度竹叶黄酮具有升高血清HDL-C 浓度的作用;
实验结果对竹叶黄酮降脂产品的开发提供必要的理论依据。
⑵本发明采用本公司【一种超声波-微波辅助复合溶剂二次重结晶及蒸馏协同精制组合提取二十八烷醇的制备方法(专利申请号:202210303916.9)】所述的从新鲜的甘蔗滤泥中提取纯度为≥98%的二十八烷醇,是一种具有抗疲劳生理活性的功能性物质,具有抗疲劳、增强耐力和体力、改善心肌功能、 降低血脂等多种生理作用,是一种很好的天然保健功能因子:
①具有提高体育运动的功能,比如可增强耐力和体力,提高肌肉的力量,减轻肌肉疼痛,减少肌肉摩擦,缩短肌神经反应时间;
②具有改善人体生理功能的作用,主要表现为 :增进精力(包括反应灵敏性、应激能力);提高反应灵敏性 ;提高应激能力;强化心脏机能和氧气运送力、降低收缩期血压;提高机体新陈代谢的比例等;
③可提高运动性疲劳机体的血糖、血清睾酮水平,防止心肌损伤;
④能够提高机体的免疫功能,抑制胆固醇的生物合成,有助于机体在缺氧条件下的耐受性,提高氧的输送能力,提高机体在高原条件下的作业能力。
⑤减轻心脑组织血管轻度扩张、细胞水肿,对组织细胞的结构有一定保护作用,还具有潜在的抗炎、抗肿瘤功效;
⑥促进激素作用,改善对人体的生殖障碍;
⑦减少血液过多钙质和脂肪含量,是降血钙素形成促进剂,可用于防治血钙过多骨质疏松症、高胆固醇和高脂蛋白血型疾病;
⑧可用于防治老年初其帕金森氏病;
本发明经实验研究发现并验证了二十八烷醇纯度对尾吊模拟失重大鼠,其失重生物效应的影响:
众所周知,在失重条件下航天员体内发生一系列生理和生化变化,诸如血液粘滞性增加、血脂升高和骨钙丢失等;
本实验将大鼠随机分成3组:尾部悬吊组(下称A组)、尾吊加常规市场纯度为80%的二十八烷醇(下称B组)和尾吊加本发明采用的纯度为≥98%的二十八烷醇组(下称C组);每组8 只大鼠,供给量每鼠每天25mg/kg体重,实验期14d;在实验结束日,大鼠禁食12h后采集血液和组织样品;心脏穿刺采集心脏血,断头后收集躯干血,摘取胸腺和脾脏并称重,分离和摘取左侧后肢股骨;观察免疫器官的重量、红血细胞膜的流动性和股骨的生物力学性能等:
⑴胸腺和脾脏重量
B组大鼠的胸腺和脾脏的重量显著低于A组大鼠,但C组大鼠的胸腺的重量为0.37g,显著高于B组大鼠0.24g;
结果表明本发明采用的纯度为≥98%的二十八烷醇能抑制因悬吊模拟失重引起的胸腺萎缩,胸腺和脾脏是机体的重要免疫器官,这提示本发明采用的纯度为≥98%的二十八烷醇对因悬吊模拟失重引起的免疫功能下降有一定的防护作用;
⑵红细胞膜流动性
红细胞膜流动性通常用红细胞膜的荧光偏振度P值来表示,P值越大,表示烃链活动性越小,膜流动性愈小,血液微粘滞性愈大;反之,膜流动性愈大,血液微粘滞性愈小。悬吊14d之后,B组和C组两组大鼠红细胞膜的P值平均值分别为0.28和0.32,显著高于A组大鼠的0.26,C组大鼠血液的粘滞性与B组大鼠相比有降低的趋势;
⑶股骨生物力学参数 
表2    股骨三点弯曲试验力学参数(平均值)
表2给出股骨经三点弯曲试验得出的生物力学测定值。尾吊14d后,C组大鼠股骨的最大载荷、弹性极限载荷显著高于A组和B组。结果表明,本发明采用的纯度为≥98%的二十八烷醇能显著对抗悬吊大鼠股骨生物力学特性的下降;
表3     大鼠股骨生物力学性能(平均值)
表3给出从股骨生物力学和几何参数计算得出的股骨生物力学性能数据结果表明,本发明采用的纯度为≥98%的二十八烷醇组能显著改善悬吊大鼠股骨的生物力学性能;
综上实验表明,本发明采用的纯度为≥98%的二十八烷醇对尾吊大鼠具有以下功能:①显著增加胸腺重量;②改善模拟失重大鼠红细胞膜的流动性;③显著改善股骨生物力学性能;本发明采用的纯度为≥98%的二十八烷醇能够有效对抗尾吊大鼠的某些不良作用;在整个实验过程中,未观察到二十八烷醇的副作用;说明宇航员在失重情况下体内发生的一系列生理和生化变化,可以通过服用添加了本发明采用的纯度为≥98%的二十八烷醇的保健饮料或食品,利用其能够提髙运动耐力、降低血脂、改善血液粘滞性,提高缺氧耐力和预防骨质疏松的性能,有可能成为航天员的保健饮料或食品成分。
⒊本发明采用的去氘水为氘含量25~100ppm,在疾病防治和饮料用水中的应用
在自然界中,氘的含量是氢的1/7000,自然界水的氘含量一般在145-150ppm,海水的氘含量是155ppm,而冰川水的氘含量138-140ppm左右。其实,去氘水就是利用现代技术将氘降低至10-130ppm的水;
随着如今越来越多高碳水食物进入体内,加上经常熬夜、宵夜酗酒、胡吃海喝,长期缺少运动等不健康的生活方式,导致现代人细胞内存在过多的有害物质,就是“氘”。 氘在体内具有累积作用,很难自行代谢出去,它对人体的DNA、遗传、代谢以及酶系会造成许多不良影响;
喝去氘水的好处,国外已经有非常多的研究,证明去氘水的生物学效应,是近年国外核医学领域和水生理学领域对去氘水应用研究的重大突破:
⑴日本去氘水研究会研究表明:去氘水环境,能阻碍癌细胞的代谢,诱发其死亡,同时药物和机体免疫力对癌细胞的攻击也会生效;
⑵美国DDCENTER去氘研究中心实验发现:饮用去氘水可以提升静息代谢率,减缓疲劳;
⑶在美国专家LÁSZLÓ G. BOROS教授著作的《癌症防治-去氘水的生物学效应》一书中,论证了氘对调节生物代谢的意义,并在临床试验中展现了去氘水在肿瘤防治中的积极效用,还发现:低氘环境对糖尿病治疗过程有积极影响,帮助患者更好地控制血糖水平;
⑷匈牙利HYD癌症研究与药物开发机构已获得去氘水2期临床试验的伦理批准,发现去氘水可适应应用于***癌、乳腺癌、肺癌、胰腺癌等其他肿瘤的辅助用品;
⑸在2012年的《毒理学快报》中刊登了去氘水的抗衰老作用的研究报告,其结果表示去氘水逆转了锰(Mn)暴露引起的寿命缩短问题,恢复了线虫中对寿命延长有重要作用的DAF-16和SOD-3的水平;
⑹在2016年的《行为脑研究》中刊登了高氘可能增加抑郁症发病率的研究报告,研究发现:去氘水增加了觉醒的EEG指数和REM睡眠持续时间,消除了典型的抑郁状态行为,去氘水可能为抑郁症提供新的预防策略;
如高加索地区著名的长寿村罕萨,几乎没人得癌症、心脏病、血压异常等现代人常见的疾病。经调查发现:当地的日常饮用水及作物浇灌,氘含量均低于133ppm,远低于平原地区的150ppm和赤道地区的155ppm;
对于生酮饮食者、减肥塑型者,喝去氘水也是一项能帮助达到成效的选择。
用去氘水制成非酒精饮料,如:饮用水、矿化水、磁化水、软饮料和功能饮料等,能改善人类健康和生活质量。目前美国、俄罗斯、匈牙利、乌克兰、日本、德国、法国等均有去氘水产品上市,低氘水已经在各类代谢疾病、癌症中应用;
总之,水是生命之源,水中氘元素的含量是衡量水好坏的重要标准,去氘水不仅应用于科学研究,去氘水能活化免疫细胞、改善机体基础代谢水平、抗细胞突变和延缓衰老等功能,更有益于生命体的生存发展和繁衍,对于人类的健康具有重要意义。
⒋本发明采用水溶性膳食纤维,减糖代糖的另类创新解决方案
尼尔森的一项数据显示,近一年Z世代付费增多的五大产品类型中,低脂/低卡/低糖的产品排名第一。Z世代认为食品饮料不应该成为身体的负担,他们希望吃的更健康;
从0糖气泡水的爆火,我们看到了减糖概念开始迅速扩张到面包、乳制品、巧克力糖果等多个品类。然而,尽管甜味剂能帮助减少摄入糖,却仍然在一定程度上牺牲了产品口味。如何才能健康减糖,但不牺牲口味?这将成为品牌在未来打造减糖产品时必须解决的问题;
⑴本发明使用水溶性膳食纤维技术替代糖分的解决方案
本发明采用的水溶性膳食纤维,既是一种优质的水溶性膳食纤维,又是一种独特的低热量填充剂;将糖替换成膳食纤维,减少碳水含量和卡路里,应用的植物性一对一糖替代品;它不仅是天然纤维的良好来源,而且不使用任何掩蔽剂,也无后余味,具有与普通糖相同的风味;
⑵根据不同消费者的喜好和感知,调整方案,可以起到平衡和提升整体风味及口感体验的作用;   表4
①PHGG可以显著降低院内流感的发生率
自2019年底新冠病毒肆虐全球至今,人类与这种"凶悍的流感病毒"战斗了3年了,各种关于如何预防新冠病毒引发的"流感"及新冠肺炎的研究层出不穷,为有效控制新冠肺炎疫情提供了学术上的借鉴;
2021年4月份最新发表的一篇日本单中心回顾性队列研究文章The effect of partily hydrolyzed guar gum on preventing influenza infection(部分水解瓜尔豆胶预防流感感染的效果观察),探讨PHGG 预防流感感染的效果;结果显示:PHGG可影响肠道微环境,从而有助于降低流感的发生率;
PHGG带来的临床获益仍然在进一步研究中,目前研究发现,它除了改善肠道健康外,也可改善血糖,降低胆固醇和血脂,增强矿物质的吸收等,已被45个国家用以替代蕨糖和脂肪来生产低热量、低糖、低脂肪、低胆固醇和低盐食品。在亚洲地区,它更被用作纤维成分添加到强化纤维饮料中。
②抗性糊精
具有优异的生理功能:
㈠有助于保持正常的、健康的血糖水平和胰岛素水平,延缓和抑制小肠对糖类的消化吸收,并改善末梢组织对胰岛素的感受性,降低对胰岛素的需求;
相关研究表明,每日摄入一定量的抗性糊精可以有效防止糖尿病的症状;
㈡改变消化道激素的分泌和肠道内消化酶活性,抑制糖类的消化与吸收,从而起到降低血糖的作用。连续摄入这种低分子量水溶性膳食纤维,可降低血清胆固醇和中性脂肪浓度及体内脂肪量;
㈢可吸附胆汁酸、脂肪等而使其吸收率下降,可达到降血脂,改善各种类型高血脂症患者的脂类代谢的作用;
㈣在小肠内不被吸收,可直接进入大肠,能促进肠道有益菌群的生长、繁殖,同时抑制肠道有害微生物的生长繁殖;在大肠内发酵产生短链脂肪酸,产酸量较同等膳食纤维多,这些短链脂肪酸能阻止癌细胞的生长与繁殖;
㈤吸水膨胀能增加粪便体积,促进肠道蠕动,对于便秘、痔疮、结肠癌等疾病有良好的预防效果;
㈥助于预防龋齿功能;
到目前为止,美国抢办尔汤料公司的汤料产品、法国达能公司、雀巢公司等汤料、饮料和乳制品等产品也先后使用抗性糊精,饮料最大的生产公司可口可乐公司和百事可乐公司生产的健康饮料中也采用了此材料;
抗性糊精被美国FDA认可为GRAS物质,并且没有摄取量限制。在日本,抗性糊精作为营养强化剂得到广泛的应用,获得日本厚生劳动省认定为政府特定保健食品素材的认定。在我国,***[2012]516号函拟公布抗性糊精为普通食品可无限量的添加于各种食品中;
③改性聚葡萄糖
仅有部分参与人体的新陈代谢,其所产生的热量只有IkCal/g (4.18kJ/g);当它充当填充剂取代食品原料中的其他糖分或脂肪时,所提供的热量分别为糖类的25%、脂肪的11%。而且被摄入人体后,其代谢过程与胰岛素没有关系,故不会引起血糖变化,适合糖尿病患者食用;
根据东京大学的Tomotari Mistuoka对一些健康的志愿者进行了每日服用10g聚葡萄糖的临床研究的试验结果,表明聚葡萄糖能防止这些类固醇的重吸收;服用聚葡萄糖后,与结肠癌有关的一葡萄糖昔酶的活力下降,这说明聚葡萄糖能减少患结肠癌的风险;
   在日本,改性聚葡萄糖被认为是重要的膳食纤维米源。研究表明,青年妇女连续5日,每日喝1瓶含7~10g改性聚葡萄糖的饮料,其粪便显著***,便秘得到有效缓解; 
在一些国家如中国、日本和南韩等,改性聚葡萄糖更被视为重要的水溶性膳食纤维;
④低聚果糖
能有效降低血清胆固醇、甘油三脂、游离脂肪酸的数量,对于因血脂高而引起的高血压、动脉硬化等一系列心血管疾病有较好的改善作用。低聚果糖在大肠内被细菌发酵生成L-乳酸,可以溶解钙、镁、铁等矿物质,促进人体对矿物质的吸收。抑制有害细菌的生长,调节肠道内平衡;能促进微量元素铁、钙的吸收与利用,以防止骨质疏松症;可减少肝脏毒素,能在肠中生成抗癌的有机酸,有显著的防癌功能;且口味纯正香甜可口,具有类似脂肪的香味和爽口的滑腻感。低热能值,由于低聚果糖不能被人体直接消化吸收,只能被肠道细菌吸收利用,故其热值低,不会导致肥胖,间接也有减肥作用。对糖尿病患者来说也是一种良好的甜味剂;
实验证实,低聚果糖促进钙的吸收率达70.8%。因此,低聚果糖可以促进生长发育和防止骨质疏松症;同时还可促进维生素B1、B2、B3、B6、B12及叶酸的自然形成,从而提高人体新陈代谢水平,提高免疫力和抗病力。预防及改善由于体内毒而引起的皮肤性疾病,可防止面疮、黑斑、雀斑,青春痘、老人斑,使皮肤亮丽、老化减缓。双歧杆菌吸收低聚果糖后,迅速增殖,抑制大肠杆菌、沙门氏菌和梭状芽胞杆菌等腐败菌发生作用,减少毒性代谢物(如吲哚、亚硝基氨)的生成,同时迅速将毒性代谢物排出体外,减轻肝脏负担,起到保护肝脏的作用,预防各种慢性病、癌症等作用明显;低聚果糖极少会被消化道中的胃酸和酶分解,极难被人体吸收;
根据测定,低聚果糖的热值为1.5Kcal/g以下,而蔗糖热值为4.6Kcal/g,因此摄入低聚果糖后,不会引起肥胖,是理想的低热值的功能性甜味剂。低聚果糖不能被突变链球菌利用生成不溶性葡聚糖而提供口腔微生物沉积、产酸和腐蚀的场所(牙垢) ,因此可以防止龋齿。
⒌本发明采用的另类乳化、稳定解决方案
本发明经实验研究发现并验证了: 各因素对一种超高纯度二十八烷醇-黄酮复合无氘水组合协同精制的高能饮料稳定性的影响:
⑴乳化剂对饮料稳定性的影响 
乳化剂种类和用量的选择,在稳定乳化液体系的形成过程中起着重要的作用;适宜的乳化剂可以显著降低两相间的表面张力,改变体系的界面状态,有利于稳定液滴的均匀分散;
①单因素油溶性乳化剂对饮料稳定性的试验
油溶性乳化剂选取司盘80为例,进行实验,考察其用量对饮料的稳定作用;
表5  油溶性乳化剂对饮料稳定性的影响结果
②单因素水溶性乳化剂对饮料稳定性的试验
水溶性乳化剂选取吐温80为例,进行实验,考察其用量对饮料的稳定作用;
表6  水溶性乳化剂对饮料稳定性的影响结果
③复配乳化剂对饮料稳定性的影响
为了提高乳化效果,选取油溶性乳化剂司盘80(A)、水溶性乳化剂吐温80(B)两个因素的不同水平组合进行双因素等重复试验为例,A的浓度取0.05份、0.1份、0.15份三个水平,B的浓度取0.10份、0.15份、0.2份三个水平。以离心沉淀率(%)为检验标准,离心沉淀率越小越好。试验结果见表3:
表7  双因素等重复试验数据及计算表
由表7结果表明,可确定最佳组合水平为0.2份吐温80、0.1司盘80时,饮料的离心沉淀率最小。因此上述组合配方制的的饮料能达到最好的乳化;
⑵稳定剂对饮料稳定性的影响 
①多种稳定剂的单因素试验
本实验分别选取了3种常用亲水胶体:黄原胶、羧甲基纤维素钠(CMC)、***胶作为稳定剂进行体态稳定性的单因素试验为例,在相同条件下观察饮料从静止到出现大量沉淀,根据稳定效果来确定最终试验所需稳定剂的种类;
表8  多种稳定剂的单因素试验
由表8可以看出,黄原胶、羧甲基纤维素钠(CMC)、***胶这3种稳定剂单独作用于饮料时效果较好,其中黄原胶的效果最好,符合它自身增稠作用最强的特点;
②几种稳定剂复配对饮料稳定性的影响
在单一稳定剂对比试验中,各种稳定剂均未达到理想效果,因此,本实验进一步采用复合稳定剂进行试验。根据单因素试验结果,以黄原胶(0.4份、0.6份、0.8份)、羧甲基纤维素钠CMC(0.2份、0.4份、0.6份)、***胶(0.2份、0.4份、0.6份)这三种为稳定剂影响因素,进行正交试验,以离心沉淀率为指标,确定最佳配比、用量。测定沉淀率时每个处理重复3次取平均值。试验设计结果见表9
表9  复配稳定剂的确定正交试验结果
由表9可以看出,稳定剂的最佳组合为黄原胶0.6份、羧甲基纤维素钠CMC 0.2份、***胶0.4份时,饮料的离心沉淀率最小;因此,上述组合配方制的的饮料能达到最好的稳定性;
黄原胶作为增稠剂、乳化剂、稳定剂,因具有假塑性,可增加饮料的浓厚感,并稳定各成分的悬浊性,增稠但无黏糊感,并有良好的放香性;***胶作为饮料中的乳化助剂,具有很好的水溶性和乳化性食品粘着剂,在包埋过程中可以使包埋物的效率增加,加强口感,防止沉淀保持香味的护囊剂;羧甲基纤维素钠(CMC)具有增稠、悬浮、乳化、稳定等多种功能,具有较好的保水性、分散性、触变性,并可以在运输和存储过程中控制冰晶的大小和生长,用于饮料作保护剂;所以,上述三者组合可防止饮料凝聚;
⑶其他因素对饮料稳定性的影响
①高速剪切条件对饮料稳定性的影响
高剪切乳化速度对饮料稳定性的影响也是较为显著的。试验表明,搅拌速度很低时,饮料乳化效果较差,有明显的上浮分层现象,随着搅拌速度的不断升高,饮料的稳定性呈正比增长的趋势,但当乳化速度达到1.8x104r/min后,增长渐渐趋缓;
综合以上因素,选取1.8x104r/min为最佳乳化速度;乳化时间过短,乳化过程不够充分,饮料上浮现象也较严重;当乳化过程基本完成之后,延长搅拌时间对稳定性提高的幅度极小,在实际生产中价值不大,所以乳化时间以25min为宜;
②均质条件对饮料稳定性的影响
均质是防止饮料产生沉淀和分层的常用物理方法,均质温度和压力的选择直接影响到均质的效果。在本试验中采用压力为30-35Mpa,温度为60-70℃对饮料进行均质处理,试验表明:当压力在30-35Mpa,温度在60-70℃,均质两次时产品无分层、上浮、沉淀现象。从实验中还可以看出,压力越大,温度越高,均质次数越多,颗粒越细腻,但温度、压力过大。均质次数过多会过多耗用生产成本。因此,选用压力30-35Mpa,温度60-70℃,均质两次,第一次均质3至4min,间隔25min;第二次均质1至2min,经电子显微镜检测后明显可见直径为 3μm~5μm的水包油型液滴。可以生产出品质良好,组织形态好而稳定的饮料;
各种因素对饮料稳定性影响的主次顺序依次为:高剪切乳化时间>水溶性乳化剂用量>油溶性乳化剂用量>稳定剂用量;
③产品稳定性的影响
㈠体系灭菌
UHT,105-121℃,6-10秒;可以达到较好的杀菌效果,且不会使饮料性状产生明显的变化;但超过或采用长时间的加热方式进行杀菌,会产生溶质分层上浮现象;
㈡储藏稳定性
分别釆用37℃、4℃、常温三个储藏条件,37℃、4℃储藏时间为2周,常温保藏 30天,实验结果显示无上浮及沉淀出现,口感也无明显变化,表明该饮料工艺配方稳定,具有较好的储藏稳定性。
⑸“颠覆” 高能饮料结构
打破常规,才是技术创新的直接思路。通过洞察消费者需求,创新改变后高能饮料结构,在带来新式健康解决方案的同时,也提升了消费者的体验感:
①【一种超声波-微波辅助复合溶剂二次重结晶及蒸馏协同精制组合提取二十八烷醇的制备方法(专利申请号:202210303916.9)】所述的从新鲜的甘蔗滤泥中提取纯度为≥98%的二十八烷醇和【一种超临界-微波辅助超微细匀浆负压空化高压组合一步法强化提取竹叶总黄酮的制备方法(专利申请号:202210302314.1)】纯度为≥95%的竹叶黄酮,均为本公司发明拥有,类似超高纯度及技术,该方面尚未见报道;
基于业界公知认知,纯度决定一个药物的生理活性,黄酮和二十八烷醇的纯度至少要达到90%,才能达到有效降脂、预防心血管等疾病的效果,本发明采用的纯度为≥95%的竹叶黄酮和的纯度为≥98%的二十八烷醇,在饮料中,不仅可用于抗疲劳和提高人体机能的保健作用,还进一步拓展了其预防疾病等领域的进一步发展;
本发明提出以一种超高纯度二十八烷醇-黄酮复合无氘水协同组合,根据各提取物的特点,进行的交叉对比及集成,合理有效的大大强化、提高精制的高能饮料对机体调节互补、协同的作用,利于吸收和体内循环;其将超高纯度提取物引入饮料,改变了被动补充的观念,创建了主动调理饮料的制作观念,在抗疲劳、提高人体机能的保健、美容减肥等作用上具有更加优越的效果,进一步拓展了其预防疾病等领域的发展;根据实际需要,通过调节组分的变化,用作于保健、新一代运动饮料、潜水员、航天员和军队开发军需高能饮品等领域,该方面尚未见报道;不仅令人耳目一新,为更好地开发高能饮料提供理论参考,将成为今后高能饮料的制作理念,而且将越來越受到社会的关注;对于丰富我国新一代功能性高能饮料及促进人类的健康事业的发展,具有重要的现实意义;因此,本发明将有着极其广阔和实用的价值;
②本发明解决了二十八烷醇和黄酮水溶性差的问题,其在饮料中不会产生任何风味及感观的问题,均一性较好;
③本发明采用水溶性膳食纤维,减糖代糖的另类创新解决方案;
④选用的材料,为清真认证原料制成,无宗教区分;无糖、无色素,绿色、纯净、健康,这也为清真高能饮料提供了质量和安全保障;
⑤本发明精制工艺流程操作相对简单、省时。
下面结合实施例对本发明作进一步说明:下面结合实施例对本发明提供的技术方案进行详细的说明,但是不能把它们理解为对本发明保护范围的限定。
附图说明
图1为本产品竹叶黄酮提取纯度检测报告。
图2为本产品竹叶黄酮提取纯度检测报告结果。
图3为本产品从新鲜的甘蔗滤泥中提取二十八烷醇纯度检测报告。
图4为本产品从新鲜的甘蔗滤泥中提取二十八烷醇纯度检测报告结果。
本发明的最佳实施方式 实施例
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
所述的黄酮为纯度≥95%的竹叶黄酮;
所述的去氘水为氘含量25~100ppm。
其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水100ppm1000份、水溶性膳食纤维15份玉米淀粉抗性糊精加入密封反应釜内,开启搅拌,转速为500r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.1份、黄酮0.2份、稳定剂0.6份黄原胶、0.2份羧甲基纤维素钠CMC、0.4份***胶、复配乳化剂0.2份吐温80、0.1份司盘80,同时加热至85℃,在1.8x104r/min的高剪切速度下乳化25min;降温至70℃,再利用均质机经压力35Mpa,均质两次,第一次均质4min,间隔25min;第二次均质2min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.25份羟基苯甲酸酯类、酸味剂0.2份柠檬酸加入步骤⑴中的基料,转速为500r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,10秒;
⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
本发明的实施方式 实施例
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
所述的黄酮为纯度≥95%的竹叶黄酮;
所述的去氘水为氘含量25~100ppm。
其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水50ppm950份、水溶性膳食纤维20份部分水解瓜儿豆胶(PHGG)加入密封反应釜内,开启搅拌,转速为400r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.05份、黄酮0.2份、稳定剂0.17份鱼明胶、0.03份魔芋胶、复配乳化剂0.15份蔗糖脂肪酸酯、0.1份单硬脂酸甘油酯,同时加热至85℃,在1.8x104r/min的高剪切速度下乳化25min;降温至65℃,再利用均质机经压力33Mpa,均质两次,第一次均质3.5min,间隔25min;第二次均质1.5min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.3份山梨酸钾、酸味剂0.1份苹果酸为加入步骤⑴中的基料,转速为400r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,8秒;
⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
实施例
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
所述的黄酮为纯度≥95%的竹叶黄酮;
所述的去氘水为氘含量25~100ppm。
其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水25ppm900份、水溶性膳食纤维25份改性聚葡萄糖加入密封反应釜内,开启搅拌,转速为300r/min,在常温下,搅拌至完全溶解后;加入0.15份二十八烷醇、0.12份黄酮、稳定剂0.3份***胶、复配乳化剂0.045份分子蒸馏单甘酯、0.045份蔗糖脂肪酸酯、0.18份Tween60,同时加热至85℃,在1.8x104r/min的高剪切速度下乳化25min;降温至60℃,再利用均质机经压力30Mpa,均质两次,第一次均质3min,间隔25min;第二次均质1min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.03份乳酸链球菌素、酸味剂0.05份乳酸加入步骤⑴中的基料,转速为300r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,6秒;
⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
对照例1-1
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
所述的黄酮为纯度≥20%的竹叶黄酮;
所述的去氘水为氘含量25~100ppm。
其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水100ppm1000份、水溶性膳食纤维15份玉米淀粉抗性糊精加入密封反应釜内,开启搅拌,转速为500r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.1份、黄酮0.2份、稳定剂0.6份黄原胶、0.2份羧甲基纤维素钠CMC、0.4份***胶、复配乳化剂0.2份吐温80、0.1份司盘80,同时加热至85℃,在1.8x104r/min的高剪切速度下乳化25min;降温至70℃,再利用均质机经压力35Mpa,均质两次,第一次均质4min,间隔25min;第二次均质2min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.25份羟基苯甲酸酯类、酸味剂0.2份柠檬酸加入步骤⑴中的基料,转速为500r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,10秒;
⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
对照例1-2
一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥80%的二十八烷醇;
所述的黄酮为纯度≥95%的竹叶黄酮;
所述的去氘水为氘含量25~100ppm。
其制备方法,包括如下步骤:
⑴按照重量份配比称取去氘水100ppm1000份、水溶性膳食纤维15份玉米淀粉抗性糊精加入密封反应釜内,开启搅拌,转速为500r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.1份、黄酮0.2份、稳定剂0.6份黄原胶、0.2份羧甲基纤维素钠CMC、0.4份***胶、复配乳化剂0.2份吐温80、0.1份司盘80,同时加热至85℃,在1.8x104r/min的高剪切速度下乳化25min;降温至70℃,再利用均质机经压力35Mpa,均质两次,第一次均质4min,间隔25min;第二次均质2min,得到稳定的基料;
⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.25份羟基苯甲酸酯类、酸味剂0.2份柠檬酸加入步骤⑴中的基料,转速为500r/min,继续搅拌30min;
⑶体系灭菌:UHT,105-121℃,10秒;
⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
对比实验1
为观测高能饮料对大鼠血清高密度脂蛋白胆固醇浓度的效果,特将实施例1与对照例1-1进行对比实验,通过检测大鼠的血清高密度脂蛋白胆固醇(HDL-C)水平指标,为高能饮料的提高密度脂蛋白胆固醇(HDL-C)的功效给出具体数据参考:
选取大鼠, 提供基础饲料, 自由饮水、饮食; 饲养室室温为23±5℃, 相对湿度为 40%~70%, 照明随同自然变化。动物观察适应5d后, 选取80只进行实验, 随机分为4组,将其中3组改喂混合型高脂动物模型饲料:在基础饲料中添加20%蔗糖、15%猪油、1.2%胆固醇、0.2%胆酸钠,6.6%酪蛋白、0.5%磷酸氢钙、0.3%石粉,并将3组中的2组小鼠的饮用水替换成实施例1制备的高能饮料、对照例1-1制备的高能饮料。每周称重1次、记录进食量并计算食物利用率,试验持续30天。于实验中期不禁食眼球采血,测定血清HDL-C。实验末期,大鼠不禁食眼球采血,测定血清中HDL-C。解剖观察,留取肝脏、脾脏、肾脏、睾丸、肾周脂和睾周脂称重,计算相应指数。采用SPSS16.0软件统计分析数据。数据以均值±标准误差(∑±s)表示,显著性检验采用单因素方差分析,数据间比较采用t检验方法。结果如下:
表10  对大鼠血清LDL-C浓度的影响
从结果上来看本发明采用的纯度为≥95%竹叶黄酮时,可显著提高试验大鼠血清HDL-C浓度,采用纯度为20%的竹叶黄酮时,提高血清HDL-C浓度不明显(表10)。研究表明,本发明添加高纯度竹叶黄酮时,具有显著升高血清HDL-C 浓度的作用。
对比实验2
为观测高能饮料的提取物不同纯度对提高小鼠游泳时间,抗抗疲劳作用的效果,特将实施例1与对照例1-2进行对比实验,取大鼠30只,随机分为实施例1制备饮料(下称饮料A组)、对照例1-2制备饮料(下称饮料B组),去离子水空白对照组(下称C组)、每组10只,对小鼠灌胃给药,每只10ml,给药剂量相当于3g/kg,连续给药15天并于末次给药后30min:
①爬杆试验和负重游泳试验
将经训练筛选过的小鼠分别放在垂直悬挂的光滑玻璃棒上端,使其肌肉处于静力紧张状态,记录小鼠从爬杆开始,直至肌肉疲劳,无力抱住玻璃棒而落到地上的时间,反复3次,第三次跌落后终止试验,累计3次的时间作为爬杆时间(s);
各组继续灌胃给药 5d,末次给药后 30min,按体重的 8%在其尾根以铅丝负重;将小鼠置于常温的游泳箱中,记录小鼠自游泳开始至死亡的时间,作为游泳时间(min);
去离子水空白对照组实验:对小鼠灌胃给去离子水,每只10ml,给药剂量相当于3g/kg,连续给药5天并于末次给药后30min进行负重游泳,常温水,按体重的 8%在尾部负重铅皮,游泳直至力竭,沉入水中不起10s不起,记录时间;
对运动耐力的影响,经实际测试结果如下:
表11  各试验组对小鼠耐力的影响   (平均值)  
②对游泳后生化指标的影响
灌胃给药15d时,于给药后30min,按小鼠体重的3%在其尾根部以铅丝负重,在常温水中游泳30min后取出,去除负重,安静15min后眶上静脉丛取血,用对羟基联苯显色法测定血乳酸含量;
各组小鼠继续灌胃给药5d,于末次给药之后30min,放入常温水中游泳60min后取出,眶上静脉丛取血,试剂盒法测定血清尿素氮。然后立即处死动物,取肝脏,以0.9% NaCl 溶液冲洗, 滤纸吸干,蒽酮法测定肝糖原含量;
②结果
表12  二十八烷醇提取物对游泳小鼠部分生化指标的影响(平均值)
灌胃 15d 的小鼠负重游泳后,A组的血乳酸显著低于B照组,说明该作用的发挥可能与受试物的纯度有关;
A组的肝糖原含量含量比B组显著增加,说明本发明采用的纯度为≥98%的二十八烷醇,能够提高动物体内糖原的蓄积能力;
灌胃给药20d的小鼠游泳后测定血清尿素氮水平,A组显著低于B组,相比差异极显著,说明本发明采用的纯度为≥98%的二十八烷醇能够显著降低血清尿素氮,提高机体耐力和对运动负荷的适应性;
上述测试,可以看到饮料A组采用的是纯度≥98%的二十八烷醇时,具有显著的抗疲劳的功效,说明本发明的高能饮料具有抗疲劳的保健效果;饮料B组采用的是低纯度的二十八烷醇,抗疲劳效果显著性明显低于饮料A组。
以上所有实施例仅用以说明本发明的技术方案,并不构成对实施方式的限制,尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对上述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换、可以想到的其他替代手段,均在本发明的保护范围之列,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
工业实用性
本领域常规技术知识及业界共识,目前国内外研究竹叶黄酮的提取技术状况:
一种经柱纯化制备竹叶黄酮提取物的方法200910223926.6显示竹叶黄酮纯度为20.78%;
一种从竹叶中提取竹叶黄酮的生产方法200610053134.5显示竹叶黄酮纯度为≥24%;
一种基于微波辅助工艺从竹叶中分离纯化黄酮和内酯的方法CN201510481490显示竹叶黄酮纯度为≥29%;
一种竹叶黄酮提取物的制备方法200910223927.0显示竹叶黄酮纯度为42%;
一种从竹叶中提取黄酮的方法201110003352.9显示竹叶黄酮纯度为30~50%;
一种提取竹叶黄酮的方法201110406495.4显示竹叶黄酮纯度为30~50%;
从竹叶中提取竹叶黄酮类系列产品的生产工艺200610053436.2显示竹叶黄酮纯度为60%;
竹叶黄酮提取物的制备方法200810195064.6显示竹叶黄酮纯度为40%-65%;
游辉等通过试验优化得到适宜的纯化工艺条件为溶液pH5.0,吸附流速然后以3BV水洗柱,再以4BV60%乙醇溶液以1.5mL-min流速洗脱。经测定,纯化后产品中黄酮含量为54.16%;
朱宏莉等将竹叶粗提物用氯仿萃取,然后将氯仿层样品过X-5大孔树脂,经高浓度醇溶液洗脱后,将一次纯化样品再过聚酷胺柱,最后,二次纯化样品中总黄酮含量可以达到78.97%;
太原理工大学-竹叶中黄酮类化合物研究进展-文显示:得到黄酮含量为24%的竹叶黄酮粉;
中南林业科技大学-竹叶黄酮提取、纯化及抗氧化活性研究-文显示:得到的产物中总黄酮含量为36%;
扬州大学食品科学与工程学院-竹叶黄酮的生理活性与应用研究-
文显示:得到的竹叶黄酮含量达到40%以上;
北京林业大学生物科学与技术学院食品系-竹叶黄酮纯化中吸附剂的优选及解析特性研究-文显示:该工艺生产的竹叶黄酮纯度达到54.16%;
南昌大学-毛竹叶活性多糖、类黄酮的中试提取-文显示:经AB-8树脂精制后的毛竹叶黄酮纯度达到79.4%;
因此,根据本领域常规技术知识及业界共识,对比文件2所描述的竹叶黄酮只是一个概念性的概括,实际上只是个粗提物,提取率低,提取中杂质较多(如酚类、皂昔类、鞭质类、生物碱类、多糖类、蛋白质、粗脂肪、叶绿素、蒽醌类化合物、菇类内酷、无机盐、水分、矿物质、灰分、重金属、砷和锰、锌、硒等微量元素、20多种矿物质元素、82 种芳香成分化合物、16种氨基酸、53 种挥发性成分、10种醇类、17种醛类等),所谓的竹叶黄酮只是这些物质的其中一部分含量,充其量只是一种商品名称。
根据本领域常规技术知识及业界共识,目前国内外研究二十八烷醇的提取技术状况:
金宝渊等研究了从长白山蜂蜡中分离制备二十八烷醇的工艺,但设备投人大,工艺复杂,收率较低,难以工业化生产。
张相年等将虫蜡熔化后,倒入***中,采用还原法用LiAIH4催化,在70~80℃还原2.5h后得到高碳脂肪醇混合物,经分子蒸馏纯化得到含二十八烷醇16.7%的少量产品。
陈芳等采用酯交换反应提取糠蜡中的高级脂肪醇,结果表明二十八烷醇得率为43.99%,二十八烷醇含量为10.98%,将混合醇进行一次分子蒸馏后二十八烷醇含量可达37.6%。
宋建华等采用混合溶剂从虫蜡中提取,收率可达9%,二十八烷醇的含量为41.3%。
王兴国等以粗糠蜡为原料,经过精制,采用超声波水解米糠精蜡、脂肪醇的提取、分子蒸馏技术分离二十八烷醇、三十烷醇,制备得到纯度大于80%的产品。
厦门大学化工厂利用四川等蜂蜡为原料,利用生产三十烷醇的剩余物提取二十八烷醇,纯度为12.8%和 18%,但由于原料及成本原因,在产量和价格上竞争力大大降低。
另外厦门大学也以虫腊为原料生产二十八烷醇,突出的缺点是成本较高,二十八烷醇含量也没有很大突破。
南昌大学环境与化学工程学院的文献【高纯度二十八烷醇的制备与应用】一文描述:以虫白蜡为原料,采用醇相皂化法制备长碳链脂肪醇,经重结晶制得高纯度二十八烷醇,采用毛细管气相色谱测定产物中二十八烷醇含量,结果表明:长链脂肪醇的平均得率为23.30%,二十八烷醇含量为39.08%。
南昌大学的文献【二十八烷醇的制备、纯化及应用研究】一文描述:描述蜂蜡制备二十八烷醇,收率低且纯度不高;虫蜡制备二十八烷醇的收率达9%,高级醇含量达97.1%,其中二十八烷醇含量为41.3%。
江南大学欧佰特食品公司用米糠蜡开发出二十八烷醇含量达50~60%的产品,并已通过中试,但受市场影响现产量不大。其它目前国内二十八烷醇生产厂家见表13
表13 国内二十八烷醇生产厂家情况
 
小麦胚芽饮料及其制备方法-201010615889.6权利要求4.所述的二十八烷醇是先采用超临界CO2萃取方法从小麦胚芽中萃取,获得二十八烷醇白色片状结晶,其中二十八烷醇含量为42.1~43.5%;
国内二十八烷醇的生产多以米糠腊为原料,产品中二十八烷醇纯度较低,属低端产品。
古巴Policosanol中所含24~34碳高级烷醇占提取物重量90%以上,其中二十八烷醇含量为60%~70%。
二十八烷醇在日本大多数是以米糠油和米胚油为提取原料,二十八烷醇的含量一般为10%~15%,系 C22~C36 脂肪醇混合物,其中多数厂家的二十八烷醇产品中二十八烷醇含量通常为 12%。
而目前国际国内大多数厂家提纯的二十八烷醇含量一般为 12%左右,系C22~C36 脂肪醇混合物。即使是日本的二十八烷醇商品其含量也只在15%左右。二十八醇的早期产品主要为小麦胚芽油浓缩物;目前,除日本在利用米糠制取二十八烷醇方面有所进展外,国外在米糠二十八烷醇的规模化生产技术方面并无优势。由于目前二十八烷醇的主要提取原料为米糠蜡、虫姑、小麦胚芽油、甘蔗蜡,由于它不溶于水,溶于有机溶剂,加之存在物的结构比较复杂,而目前这类物质上要是原料经皂化后用有机溶媒(正己烷、丙酮等)提取,得到一种白色或浅黄色粉末状品体,此粉末状晶体为天然髙级烷醇混介物(含有24-34个碳原子高级烷醇),目前该产品技术也只是含量二十八烷小于50%。二十八烷醇的常规提取纯度只能达到 15-35%,目前国外产品一般系 C22~C36 的脂肪醇混合物,二十八烷醇含量一般为 10%~15%,国内报道的最高含量为 60%,因此目前普利醇98%,二十八烷醇60%成为市场上热销规格。
因此,根据本领域常规技术知识及业界共识,对比文件2所描述的竹叶黄酮只是一个概念性的概括,实际上只是个粗提物,提取率低,提取中杂质较多(如酚类、皂昔类、鞭质类、生物碱类、多糖类、蛋白质、粗脂肪、叶绿素、蒽醌类化合物、菇类内酷、无机盐、水分、矿物质、灰分、重金属、砷和锰、锌、硒等微量元素、20多种矿物质元素、82 种芳香成分化合物、16种氨基酸、53 种挥发性成分、10种醇类、17种醛类等),所谓的竹叶黄酮只是这些物质的其中一部分含量,充其量只是一种商品名称。
不同纯度的竹叶黄酮和二十八烷醇在不同的领域起着不同的的效果。由于竹叶黄酮和二十八烷醇的纯度越高,其活性也就越强,极性越大,若想达到有效降脂、预防心血管等疾病,提高缺氧耐力和预防骨质疏松的性能等效果,纯度至少要达到90%,因此,纯度决定一个药物的生理活性;
综上所述,目前对竹叶黄酮和二十八烷醇的提取方法虽然已经有一定的成果,但目前厂家的黄酮和二十八烷醇产品中纯度均较低,而且给进一步分离带来很多麻烦,后续精制工艺流程操作相对繁琐、费时;市场上述这种纯度只能用于抗疲劳和提高人体机能的保健作用,因而限制了其在食品及医药领域的进一步发展;
因此如何从天然物高效、经济、环保的提取便是得到大量高品质此类物质在生产中应解决的问题。所以如何低成本地制备高纯度的黄酮和二十八烷醇是目前各国科学家研究的重点。
本发明采用的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;采用的黄酮为纯度≥95%的竹叶黄酮。根据各提取物特点,进行交叉及集成,将超高纯度提取物引入饮料,改变了被动补充的观念,创建了主动调理饮料的制作观念,合理有效的大大强化、提高饮料对机体调节互补、协同的作用,在抗疲劳、提高人体机能的保健、美容减肥等作用上具有更加优越的效果,进一步拓展了其预防疾病等领域的发展;根据实际需要,通过调节组分的变化,用作于保健、新一代运动饮料、航天员和军队开发军需高能饮品等领域。

Claims (8)

  1. 一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:包括以下组分:二十八烷醇0.05~0.1份、黄酮0.12~0.2份、去氘水900~1000份、稳定剂0.1-0.3份、复配乳化剂0.3份、水溶性膳食纤维15~25份、复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份;
    所述的二十八烷醇为从新鲜的甘蔗滤泥中提取纯度≥98%的二十八烷醇;
    所述的黄酮为纯度≥95%的竹叶黄酮;
    所述的去氘水为氘含量25~100ppm。
  2. 根据权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的复配乳化剂为吐温60、吐温80、蔗糖脂肪酸酯、分子蒸馏单甘酯、单硬脂酸甘油酯、司盘60、司盘80中的两种或两种以上的混合物。
  3. 根据权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的稳定剂为***胶、鱼明胶、黄原胶、果胶、羧甲基纤维素钠CMC、环状糊精、魔芋胶中的一种或两种以上的混合物。
  4. 根据权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的复配电解质为柠檬酸钠0.65份+乳酸钙0.6份+氯化钾0.37份+乳酸镁0.35份的混合物。
  5. 根据权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的水溶性膳食纤维为改性聚葡萄糖、部分水解瓜儿豆胶(PHGG)、小麦淀粉抗性糊精、玉米淀粉抗性糊精、低聚果糖中的一种或两种的混合物。
  6. 根据权利要求4所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的酸味剂为柠檬酸、苹果酸、乳酸、燕窝酸中的一种或两种的混合物。
  7. 根据权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:所述的防腐剂为羟基苯甲酸酯类、山梨酸钾、乳酸链球菌素中的一种或两种的混合物。
  8. 用于制备如权利要求1所述的一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法,其特征在于:包括如下步骤:
    ⑴按照重量份配比称取去氘水900~1000份、水溶性膳食纤维15~25份加入密封反应釜内,开启搅拌,转速为300~500r/min,在常温下,搅拌至完全溶解后;加入二十八烷醇0.05~0.1份、黄酮0.12~0.2份、稳定剂0.1-0.3份、复配乳化剂0.3份,同时加热至85℃,在1.8X104r/min的高剪切速度下乳化25min;降温至60-70℃,再利用均质机经压力30-35Mpa,均质两次,第一次均质3至4min,间隔25min;第二次均质1至2min,得到稳定的基料;
    ⑵降温至50-55℃,按照重量份配比称取复配电解质1.97份、防腐剂0.03~0.6份、酸味剂为0.05~0.2份加入步骤⑴中的基料,转速为300~500r/min,继续搅拌30min;
    ⑶体系灭菌:UHT,105-121℃,6-10秒;
    ⑷灌装:得到一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料。
PCT/CN2023/092553 2022-05-06 2023-05-06 一种超高纯度二十八烷醇-黄酮复合去氘水组合协同精制的高能饮料及其制备方法 WO2023213325A1 (zh)

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