CN110787299A - Composition and preparation method thereof - Google Patents
Composition and preparation method thereof Download PDFInfo
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- CN110787299A CN110787299A CN201911074489.6A CN201911074489A CN110787299A CN 110787299 A CN110787299 A CN 110787299A CN 201911074489 A CN201911074489 A CN 201911074489A CN 110787299 A CN110787299 A CN 110787299A
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Abstract
The invention provides a composition and a preparation method thereof. The invention discovers that caffeine has obvious synergistic dissolution promotion and stabilization effects on dihydromyricetin and a composition of dihydromyricetin and resistant dextrin (or cyclodextrin); the resistant dextrin (or cyclodextrin) has the effects of improving sensory quality (debitterizing) and enhancing stability of the composition, so that the dihydromyricetin-caffeine-resistant dextrin (or cyclodextrin) composition and the preparation process thereof are developed and provided, and the dihydromyricetin-caffeine-resistant dextrin (or cyclodextrin) composition has important industrial application values.
Description
Technical Field
The invention relates to a composition and a preparation method thereof. More particularly, the present invention relates to a composition rich in dihydromyricetin-caffeine-resistant dextrin and/or cyclodextrin and a preparation method thereof.
Background
Dihydromyricetin (DMY), also known as ampelopsin, is a white needle-like crystal that is slightly soluble in water and readily soluble in hot water, ethanol and acetone. DMY belongs to natural flavanonols compounds, is mainly derived from Ampelopsis grossedentata, is also called Ampelopsis grossedentata tea, nectar and the like, belongs to grapevine Ampelopsis plants, comprises Ampelopsis grossedentata (Ampelopsissopsissostepetata W.T.Wang) and Ampelopsis megalophylla (Ampelopsis megalophylla Diels et. Gilg) and other plants, and the DMY content in the tender leaves and the tea tips of the Ampelopsis grossedentata can reach more than 20 percent generally, so the DMY is a plant source with the highest known DMY content. Vine tea contains no caffeine or very little (negligible) caffeine. Pharmacological research shows that DMY has obvious health care and treatment effects of resisting inflammation, resisting oxidation, losing weight, reducing blood fat, reducing blood pressure, reducing blood sugar, protecting liver and the like, and has important application value.
The DMY composition drink is one of the important research and development contents of the invention. The beverage (especially liquid beverage) is a product formulation which is popular with consumers and has better industrial application value.
It is very necessary to develop a beverage with higher concentration of DMY. Because the clinical (health care) effective dose of DMY usually needs more than 500mg per day, and the functional health care (or treatment) drink usually needs to be drunk for a long time according to a certain effective dose, the development of DMY drink with higher concentration and smaller volume (specification) is necessary and the best choice, such as liquid drink with 10-300ml per bottle (jar), or solid drink with small specification, and the like, has important health care treatment and market application value.
However, developing higher concentration DMY beverages requires overcoming the "three-diff" problem of DMY: poor solubility, poor taste (bitter taste), and poor stability (susceptibility to oxidative browning and precipitation). These problems are important obstacles to the development of DMY beverages. Such poor solubility of DMY, whether in liquid or solid form, is clearly not conducive to the dissolution and absorption of DMY.
DMY is known to have poor water solubility, only about 0.07% (0.7mg/ml) at room temperature (Benguo Liu, et al, JFood biochemistry.2012, 36: 634; Shezhiying et al, university of Wuxi, 2004, 23 (2): 17.), and even worse at low temperatures. DMY pure powder is insoluble in water, can be gradually dissolved only by heating to a higher temperature, but is unstable after cooling, and is easy to precipitate or crystallize.
DMY is rich in phenolic hydroxyl and has remarkable antioxidant activity, but is easily affected by oxygen, high temperature and other environmental factors in the beverage to cause browning. The DMY browning refers to a process that the color of the DMY is gradually deepened from colorless (or light yellow) to brown or brown in an aerobic environment, and the essence is that the DMY undergoes an oxidative denaturation reaction, so that the content of the DMY is reduced, and oxidation products of the DMY are easy to aggregate and precipitate, and cause a series of adverse reactions such as abnormal mouthfeel.
Caffeine (cafeine, CAF), also known as 1, 3, 7-Trimethylxanthine (1, 3, 7-Trimethylxanthine), has a molecular weight of 194, is easily soluble in water and bitter in taste, is a central nervous stimulant, can refresh and resist fatigue, and is clinically used for treating neurasthenia and coma resuscitation. The caffeine is mainly derived from coffee, tea, guarana fruit, cocoa, etc. Coffee, tea, soft drinks and energy drinks containing caffeine are sold very well all over the world.
Guarana Extract (also called Guarana essence) is a soluble Extract rich in caffeine and derived from seeds of Guarana (Paulina cupana) fruits, wherein the caffeine content has various specifications (usually 5% -22%). Guarana extract has been widely used in foods and functional foods (beverages) as a food additive. Guarana, also known as Pacific cocoa, belongs to evergreen vine of Sapindaceae, is widely cultivated in the Paimason basin of Brazil, mainly produced in America, and especially in some areas of the Lonicera tropicalis of the Amazon plateau (mainly located in Brazil and Venezuela) and Paraguay and Uyghury. Guarana is known as "national drink" in brazil and is considered as the source spring bestowing youth, beauty and health and longevity by Indian people in amazon drainage basin for hundreds of years. The guarana is rich in caffeine, amino acids, tannic acid, proteins, vitamins, minerals, etc., and has effects of refreshing brain, nourishing yin, tonifying yang, controlling appetite, relieving abdominal pain, restoring physical strength, supplementing energy, and improving human body function.
Resistant Dextrin (RS) is low-molecular soluble dietary fiber processed by starch, belongs to glucan which is difficult to digest by human digestive enzymes, has the health-care effects of improving the environment of intestinal flora, reducing blood fat, resisting constipation and the like, is widely used in food and health-care products, and is safe and effective. The resistant dextrin and the DMY composition have better complementary and synergistic health care effects.
Cyclodextrin (CD) is a cyclic oligomeric glucose, is generally formed by polymerizing 6-12 glucose molecules by α -1, 4-glycosidic bonds, is commonly formed by polymerizing α -Cyclodextrin, β -Cyclodextrin and gamma-Cyclodextrin which are respectively 6, 7 and 8 glucose units, has an inclusion effect on certain small molecules, belongs to a food additive, and is generally higher in solubility.
In conclusion, the dihydromyricetin-caffeine-resistant dextrin/cyclodextrin (DMY-CAF-RS/CD) composition and the preparation process thereof according to the present invention are not available at present.
Disclosure of Invention
The invention aims to provide a DMY-CAF-RS/CD composition with better solubility and better quality and a preparation process thereof.
The inventor has intensively studied and surprisingly found that:
CAF can increase the solubility and stability of DMY dose-dependently and synergistically (see figure 1). It is known that DMY has only about 0.7mg/ml solubility in water at room temperature (20 ℃), has lower solubility at low temperature, tends to form precipitates or crystals at higher concentration, has adverse effects on stability of beverage properties and taste, and particularly has a larger amount of precipitates at low temperature, and does not meet the requirements for suitability of beverages at normal temperature and low temperature. The inventor researches and discovers that when a proper amount of CAF is added into a high-concentration DMY aqueous solution (such as 10mg/ml), the precipitation amount of DMY is reduced along with the increase of the concentration of CAF, namely, DMY and CAF are in negative correlation. Generally, when the content ratio of DMY to CAF is DMY/CAF 10, the amount of DMY solution precipitated is greatly reduced, when DMY/CAF 5, the amount of DMY precipitated is already small, and when DMY/CAF 2.5, the amount of DMY precipitated can be substantially eliminated; DMY has lower solubility in low-temperature environment (such as 4 ℃), and CAF has more prominent dissolution promotion effect, and can be used as representative conditions for research. The amount (concentration) of the CAF promoter can be adjusted appropriately according to the DMY concentration.
CAF can dose-dependently, synergistically increase the solubility and stability of DMY-RS compositions (see FIG. 1). For example, addition of 6% RS to an aqueous DMY solution (10mg/ml) precipitated more precipitate (compared to a 10mg/ml DMY solution), suggesting that both have a solubility antagonistic effect; however, if proper amount of CAF is added into the DMY10mg/ml-RS 6% combined aqueous solution, the CAF can synergistically increase the solubility of DMY and RS in a dose-dependent manner, and obviously reduce the precipitation amount of the solution. In contrast, CAF has no significant effect on the solubility of RS. The amount (concentration) of the CAF promoter can be adjusted appropriately according to the concentration of DMY and RS.
For example, the amount of the added gamma-CD needs more than 2 times that of DMY to greatly reduce the precipitation amount of a DMY10mg/ml aqueous solution, and under the condition that the amount of the added gamma-CD is not enough, such as a DMY10 mg/ml-gamma-CD 10mg/ml aqueous solution, a large amount of precipitate still can be precipitated, however, after the CAF is added, the CAF can greatly reduce or even eliminate the precipitation of the DMY-gamma-CD aqueous solution in a dose-dependent manner, and shows good synergistic solubilization, namely, the addition of a small amount of CAF can greatly promote the solubilization effect of the gamma-CD on the DMY, and the CAF also has similar synergistic solubilization effect on the DMY- α -CD (or β -CD) aqueous solution.
The solubilizing effect of CAF on DMY and DMY-RS (or CD) compositions, the effective dose can be set according to the ratio of DMY to CAF content (DMY/CAF), typically 0.30-30 DMY/CAF, preferably 0.60-20 DMY/CAF, more preferably 1-15 DMY/CAF.
DMY-CAF-RS (or CD) compositions have significantly better solubility and stability than DMY, including liquid and solid products.
6. The guarana extract has similar dissolution promoting and stabilizing effects on DMY compared with CAF when calculated by CAF content. It is suggested that other components of the guarana extract have no significant effect on the results.
RS has the effects of reducing the bitter taste of DMY and DMY-CAF compositions in a dose-dependent manner, improving the sensory quality and stability of the DMY and DMY-CAF compositions and the like. The ratio of the effective addition amount of RS to the DMY content (RS/DMY) is more than or equal to 1.0, preferably the RS/DMY is more than or equal to 3.0, and more preferably the RS/DMY is more than or equal to 5.0.
CD also has the effects of reducing the bitterness of DMY and DMY-CAF compositions in a dose-dependent manner, improving the sensory quality and stability of the compositions and the like, wherein the effects of gamma-CD, α -CD and β -CD are all effective, but the dose effect is different, the ratio of the effective addition amount of the CD to the content of the DMY (CD/DMY) is more than or equal to 0.50, preferably the ratio of the CD/DMY to the DMY is more than or equal to 1.0, and more preferably the ratio of the CD/DMY to the DMY is more than or equal to 1.5.
The anti-browning effect of the aqueous solution of the DMY-CAF-RS/CD composition is enhanced along with the reduction of the pH (the browning index is reduced), namely, the aqueous solution of the DMY-CAF-RS/CD composition has better anti-browning stability effect under the condition of increasing acidity (see the attached figure 2). DMY is rich in phenolic hydroxyl and is easy to be oxidized and browned to be denatured, so that the improvement of the antioxidant browning effect is important work for ensuring the health care function and the quality stability of DMY products. In the high-temperature accelerated oxidative browning test (such as heat treatment at 95 ℃ for 2 hours), in the pH neutral-acidic range, a DMY10 mg/ml-CAF2mg/ml-RS 6% (or CD 30mg/ml) aqueous composition solution is most easily oxidized and browned and aggregated and precipitated at the pH of 7, and the browning effect is gradually weakened along with the reduction of the pH. Thus, a pH of less than or equal to 7.0, preferably less than or equal to 6.0, more preferably less than or equal to 5.0, and most preferably less than or equal to 4.0, is required to reduce oxidative browning of the composition.
The stability of the DMY-CAF-RS/CD composition aqueous solution is obviously stronger than that of a DMY-CAF aqueous solution without RS (or CD), which is shown in that the browning index is obviously reduced, the character stability is better (sediment is not easy to form) and the DMY content is higher.
The invention has the beneficial effects that:
1. the CAF is originally discovered to have the characteristics of dose dependence and synergistic improvement of the concentration (solubility) of DMY and DMY-RS/CD aqueous solutions, RS and CD have the effects of reducing bitterness and improving stability on DMY, and the solubility promotion relationship among DMY-CAF-RS/CD molecules and stability influence factors are described, so that the DMY-CAF-RS/CD composition and the preparation process thereof are provided, the defects of low DMY solubility, poor stability and bitter taste are overcome, the non-obvious process technology progress is obvious, and the practical problem of DMY product development is effectively solved.
The DMY-CAF-RS/CD composition not only has the solubility and the stability which are obviously superior to those of DMY, but also has a multifunctional complementary effect on the aspect of health care or treatment functions, so that the composition has better market application value.
First aspect of the invention:
1. the invention provides a composition rich in dihydromyricetin, which is characterized by being selected from one of the following two conditions:
1) dihydromyricetin-caffeine-resistant dextrin (DMY-CAF-RS) composition, wherein the DMY content is more than or equal to 1.0mg/g, the CAF content is more than or equal to 0.050mg/g, the content ratio of DMY to CAF (DMY/CAF) is 0.30-30, and the RS content is more than or equal to 1.0 mg/g; preferably, DMY is more than or equal to 2.0mg/g, CAF is more than or equal to 0.10mg/g, wherein DMY/CAF is 0.60-20, and RS is more than or equal to 3.0 mg/g; more preferably, DMY is more than or equal to 3.0mg/g, CAF concentration is more than or equal to 0.20mg/g, DMY/CAF is 1-15, and RS is more than or equal to 5.0 mg/g.
2) Dihydromyricetin-caffeine-cyclodextrin (DMY-CAF-CD) composition, wherein DMY content is not less than 1.0mg/g, CAF is not less than 0.050mg/g, DMY/CAF is 0.30-30, and CD is not less than 0.50 mg/g; preferably, the concentration of DMY is more than or equal to 2.0mg/g, the concentration of CAF is more than or equal to 0.10mg/g, the concentration of DMY/CAF is 0.60-20, and the concentration of CD is more than or equal to 1.0 mg/g; more preferably, DMY is not less than 3.0mg/g, CAF is not less than 0.20mg/g, DMY/CAF is 1-15, and CD is not less than 1.5 mg/g.
2. The cyclodextrin in the composition comprises α -cyclodextrin, β -cyclodextrin, gamma-cyclodextrin and derivatives thereof.
3. The DMY extraction source of the composition comprises vine tea, vine tea extract, food raw materials or medicinal materials rich in DMY and extracts thereof.
4. Sources of CAF for the compositions of the invention include, but are not limited to: guarana extract, tea extract (including black tea, oolong tea, green tea, white tea, etc.), caffeine synthetic product and their compound products.
5. The pH value of the composition is not more than 7.0 when the product attribute is liquid; the pH is preferably less than or equal to 6.0; more preferably, the pH is less than or equal to 5.0.
6. The composition of the present invention may comprise, in addition to DMY, CAF, RS (and/or CD) in a specific content ratio, a food or pharmaceutical acceptable carrier, including but not limited to (1) liquid, such as water, saline, glycerin, ethanol, alcoholic beverages containing ethanol, (2) auxiliary components, such as emulsifiers, pH buffer substances, alginate jelly, pectin, sodium carboxymethylcellulose (CMC), xanthan gum, gellan gum, guar gum, carrageenan, citric acid, sodium citrate, malic acid, sodium malate, sucrose, fructose, maltitol, stevioside, (3) nutrients, such as L-carnitine, taurine, arginine, soluble proteins (peptides), vitamin B, vitamin C, vitamin E, β -carotene, calcium, zinc, selenium, etc. (4) single or compound extracts from plants and (or) Chinese medicinal materials, fruit and vegetable juices, etc.
7. The product form of the composition of the invention comprises: (1) liquid products including oral liquids, beverages, suspensions, gels and creams; (2) solid products including powders, granules, capsules and tablets.
Second aspect of the invention:
the invention provides a preparation method of a DMY-CAF-RS/CD composition, which is characterized by comprising the following process steps:
1. extracting to obtain DMY extract, wherein the DMY extract comprises DMY pure product (content is more than or equal to 98%) extracted from vine tea and other raw materials and extract with lower DMY content; and can also be purchased commercially.
2. Extracting to obtain CAF extract, including CAF pure product and crude extract extracted from CAF-rich raw material, guarana extract, and tea extract with various CAF contents; and can also be purchased commercially.
3. Mixing to obtain DMY-CAF-RS/CD composition, wherein: mixing DMY extract, CAF extract and RS (or CD) according to the composition proportion of the composition, adding proper amount of carrier if necessary, stirring and dissolving to form a complex. Preferably, the method comprises dissolving the compound at a temperature above 30 ℃ for at least 10 minutes, more preferably at a temperature of 40-95 ℃ for at least 15 minutes.
4. The product blending is characterized in that: adding a proper amount of the carrier of the invention into the composition, heating, dissolving and blending to obtain the required concentration and volume; adding a proper amount of acid or alkali to adjust the pH value to the required value, and is characterized in that the pH value is selected to be less than or equal to 7.0, wherein the pH value is preferably less than or equal to 6.0, and the pH value is more preferably less than or equal to 5.0.
5. Centrifuging or filtering the product concoction solution to remove insoluble particles, collecting clarified solution (or filtrate), and bottling according to set volume, and performing pasteurization (such as water bath at 90 deg.C for 15 min) or pre-sterilization (such as ultra-high temperature instantaneous sterilization UHT/125 deg.C for 3-8 s), and hot-filling or aseptic canning to obtain beverage.
6. For preparing solid products, after obtaining the DMY-CAF-RS/CD composition, the clear liquid (or filtrate) is collected by centrifugation (or filtration), concentrated and dried into dry powder or particles, and then prepared into powder or granules packaged quantitatively, or prepared into capsules or tablets.
7. In another preferred embodiment, DMY and other plant components are extracted by adding appropriate amount of pectinase and/or cellulase, and hydrolyzing at pH2-8 and 20-75 deg.C for at least 30 min, wherein the hydrolysis time depends on enzyme addition and temperature.
In a third aspect of the invention:
there is provided a use of the composition of the invention, including as a food beverage or ingredient thereof, a dietary supplement, a nutraceutical and a medicament.
Drawings
FIG. 1: effect of caffeine on the solubility of DMY, DMY-RS/CD (4 ℃). The ordinate represents the relative precipitation amount (%) of the solution, and the abscissa represents the CAF concentration. As can be seen in FIG. 1, CAF has dose-dependent significant solubilizing and stabilizing effects (character stability) on DMY, DMY-RS and DMY-CD.
FIG. 2: influence of pH value on browning effect of DMY-CAF-RS/CD composition aqueous solution. The ordinate is the browning index (OD410nm) and the abscissa is the solution pH. As can be seen in fig. 2, the anti-browning effect of the combined aqueous solution gradually increased with decreasing pH (lower browning index), i.e., the anti-browning effect of the composition was inversely related to the magnitude of the pH value.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Experimental procedures in the following examples, in which specific conditions are not specified, are generally carried out under conventional conditions or under conditions recommended by the equipment manufacturers. All percentages, ratios, proportions, or parts of this invention are by weight unless otherwise specified.
The content detection of the DMY, CAF, cyclodextrin, resistant dextrin and other components can be carried out by the conventional methods (including HPLC method and colorimetric method) in the known literature.
The features mentioned above with reference to the invention, or the features mentioned with reference to the embodiments, can be combined arbitrarily. All the features disclosed in this specification may be combined in any combination, and each feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose. Thus, unless expressly stated otherwise, the features disclosed are merely generic examples of equivalent or similar features.
Unless defined otherwise herein, the terms "comprises" and "comprising" are used in the present specification to define the invention, and are used in a generic and descriptive sense only and not for purposes of limitation. Any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are exemplary only. Furthermore, as used herein, the singular tense of a noun, without conflict with the context, includes the plural form of that noun; the use of plural nouns also covers the singular form of such nouns.
Example 1:
composition formula research
The method comprises the following steps: taking a proper amount of dihydromyricetin (DMY is more than or equal to 98 percent), caffeine (CAF is more than or equal to 98 percent) or guarana extract (CAF is more than or equal to 22 percent), resistant dextrin (RS, food grade) or cyclodextrin (CD, food grade), mixing with a proper amount of purified water, heating to 80 ℃ for 10 minutes under stirring for dissolving, subpackaging and sealing in screw test tubes (10 ml/piece), sterilizing in a water bath at 90 ℃ for 10 minutes, and respectively preparing DMY10 mg/ml-CAF series aqueous solution, DMY10mg/ml-RS 6-CAF series aqueous solution, DMY10 mg/ml-gamma-CD 10mg/ml-CAF series aqueous solution and the like. The test specimens were then stored at room temperature (20-30 ℃) and refrigerated in a refrigerator (4 ℃) for at least 30 days. The solubility (or character stability) of DMY and compositions thereof is evaluated as a mass or volume percentage of the amount of precipitate to the amount of solution, where low temperature solubility observations are more sensitive; the mouthfeel (bitterness) of the solution was evaluated on a person's trial.
The results show that:
1) CAF can increase the solubility and stability of DMY dose-dependently and synergistically (see figure 1). It is known that DMY has a solubility of about 0.7mg/ml in water at room temperature (20 ℃), is lower at low temperature, and tends to form precipitates at higher concentrations, which adversely affects the properties and taste of beverages, and particularly, precipitates are larger at low temperature, and do not meet the requirements for the suitability of beverages at room temperature and low temperature. The inventor researches and discovers that when appropriate caffeine is added into a high-concentration DMY aqueous solution (such as 10mg/ml), the precipitation amount of DMY is reduced along with the increase of the caffeine concentration, namely, DMY and CAF show negative correlation. In general, when the mass (concentration) ratio of DMY to CAF is DMY/CAF 10, the amount of DMY solution precipitated is greatly reduced, when D/C is 5, the amount of DMY precipitated is already small, and when D/C is 2.5, the amount of DMY precipitated can be substantially eliminated; DMY has lower solubility in low temperature environment (such as 4 ℃), and CAF has more prominent dissolution promotion effect. In conclusion, CAF was effective in promoting DMY dissolution at both room temperature and low temperature. The amount (concentration) of the CAF promoter can be adjusted appropriately according to the level of the DMY concentration. Usually, DMY/CAF is 0.30 to 30, preferably 0.60 to 20, more preferably 1 to 15.
2) CAF can increase the solubility and stability of DMY-RS compositions in a dose-dependent, synergistic manner, and is effective in both ambient and low temperature environments. For example, addition of 6% resistant dextrin to DMY in water (10mg/ml) precipitated more precipitate (compared to DMY in 10mg/ml), suggesting that both have a solubility antagonistic effect; however, when appropriate amount of CAF is added to the aqueous solution of DMY (10mg/ml) -RS (6%) combination, the solubility of DMY and RS can be synergistically increased in a CAF dose-dependent manner, and the precipitation amount of the solution can be remarkably reduced. In contrast, CAF has no significant effect on the solubility of RS. The amount (concentration) of the CAF promoter can be adjusted appropriately according to the concentration of DMY and RS. Usually, DMY/CAF is 0.30 to 30, preferably 0.60 to 20, more preferably 1 to 15.
3) For example, the amount of gamma-CD added is increased to 2-3 times that of DMY to greatly reduce the amount of DMY10mg/ml aqueous solution precipitation, and in the case of insufficient amount of gamma-CD, for example, DMY10 mg/ml-gamma-CD 10mg/ml aqueous solution still precipitates greatly, but the addition of CAF can greatly reduce or even eliminate the precipitation of the aqueous DMY-gamma-CD in a dose-dependent manner, and thus, a good synergistic solubilization effect is exhibited.
4) The solubility and stability of the DMY-CAF-RS/CD composition are obviously superior to that of DMY, and the DMY-CAF-RS/CD composition comprises the advantages of higher solubility of liquid products, easier dissolution process of solid products and the like.
5) The guarana extract has similar dissolution promoting and stabilizing effects on DMY compared with CAF when calculated by CAF content. It is suggested that other components of the guarana extract have no significant effect on the results.
6) RS has the effects of reducing the bitter taste of DMY and DMY-CAF compositions in a dose-dependent manner, improving the sensory quality and stability of the DMY and DMY-CAF compositions, and the like. The ratio of the effective addition amount of RS to the DMY content (RS/DMY) is more than or equal to 1.0, preferably the RS/DMY is more than or equal to 3.0, and more preferably the RS/DMY is more than or equal to 5.0.
7) The ratio (CD/DMY) of the effective addition amount of the CD to the DMY content is more than or equal to 0.50, preferably more than or equal to 1.0, and more preferably more than or equal to 1.5.
8) CD has the effects of reducing the bitter taste of DMY and DMY-CAF compositions in a dose-dependent manner, improving the sensory quality and stability of the compositions, and the like, and comprises gamma-CD, α -CD and β -CD which are effective, but have different dose effects.
Example 2:
composition stability study
The method comprises the following steps: referring to example 1, DMY10 mg/ml-CAF2mg/ml series aqueous solutions (pH7.0-3.0) and RS (or CD) -containing series aqueous solutions, etc., having different pH values were prepared by adjusting pH with dilute acetic acid and dilute NaOH, and then the samples were treated by a high-temperature accelerated oxidation method (95 ℃ C.. times.2 hours), cooled to room temperature, diluted 10-fold with water to measure the browning index (OD410nm), and the stability of the properties (precipitation reaction) and the content of DMY were observed.
The results show that:
1) the anti-browning effect of the aqueous solution of the DMY-CAF-RS and DMY-CAF-CD composition is enhanced along with the reduction of the pH value (the browning index is reduced), namely, the aqueous solution has better anti-browning stability effect under the condition of increasing acidity (see attached figure 2). In the pH neutral-acidic range, the DMY-CAF-RS (or CD) composition aqueous solution is most easily oxidized and browned and aggregated and precipitated at the pH of 7, and the browning effect is gradually weakened along with the reduction of the pH; wherein the anti-browning effect is obviously stronger than the pH value of 7 when the pH value is less than or equal to 6, the anti-browning effect is better that the pH value is less than or equal to 5.0, and the better that the pH value is less than or equal to 4.0.
2) The stability of the DMY-CAF-RS/CD composition aqueous solution is obviously stronger than that of a DMY-CAF aqueous solution without RS (or CD), which shows that the browning index is obviously reduced, the character stability is obviously improved (precipitates are not easy to form), the DMY content is higher, and the like. In contrast, aqueous DMY-CAF solutions are more stable than aqueous DMY solutions.
Example 3:
preparation of dihydromyricetin oral liquid
Example 4:
dihydromyricetin fruit juice beverage
Preparing mulberry and red date extract: mixing 120kg of dried mulberry, 100kg of dried red date and 5kg of citric acid with 2000kg of purified water, heating to 90 ℃ under stirring for 15 minutes, cooling, homogenizing, adding 1kg of pectinase and cellulase (activity is 1 ten thousand U/g), keeping the temperature at 50 ℃, stirring, hydrolyzing for 4 hours, heating to 90 ℃ under stirring for 15 minutes, cooling, performing pressure filtration, collecting filtrate, centrifuging or filtering to obtain about 2000kg of supernatant, wherein the supernatant is mulberry and red date extract.
Blending the beverage: 2000kg of mulberry and red date extract is taken, 16.2kg of vine tea extract (DMY is more than or equal to 98 percent), 20kg of guarana extract (CAF is more than or equal to 22 percent) and 200kg of resistant dextrin (food grade) are added under stirring, the mixture is stirred and heated to 90 ℃ for 10 minutes to be dissolved, then the temperature is reduced to 50 ℃ and the temperature is kept for 30 minutes, and the supernatant is centrifugally collected to be the composition extract. Taking the composition extracting solution, adding 1kg of VC, 1kg of taurine, 1kg of stevioside and 2kg of xanthan gum under stirring, heating to 90 ℃ for 10 minutes, stirring for dissolving, adjusting the pH to 3.8, filtering with a 200-mesh sieve, collecting filtrate, filling the filtrate into a bottle of 50ml, sterilizing in a water bath for 15 minutes at 90 ℃, cooling to room temperature, labeling, boxing, and inspecting to be qualified for later use.
Specification and content: 50 ml/bottle; DMY content of about 8mg/ml, CAF content of about 2mg/ml, RS content of about 100mg/g, pH 3.8. The mulberry and red date extract and the nutrients are added into the composition beverage, so that the taste and flavor of the product can be improved, and the nutrition and health care effects can be increased.
Example 5:
dihydromyricetin solid beverage
Preparing mulberry, red date and vine tea extract: taking 100kg of dried mulberry, 100kg of dried red date, 35kg of vine tea powder and 5kg of citric acid, mixing with 2000kg of purified water, heating to 90 ℃ under stirring, keeping the temperature for 20 minutes, cooling, homogenizing, adding 2kg of pectinase and cellulase (activity is 1 ten thousand U/g), keeping the temperature at 50 ℃, stirring, hydrolyzing for 3 hours, heating to 90 ℃, stirring, extracting for 30 minutes, cooling, performing pressure filtration, collecting filtrate, centrifuging, collecting supernatant fluid about 2000kg, and obtaining mulberry, red date and vine tea extract.
2000kg of mulberry, red date and vine tea extract is taken, 50kg of gamma-CD and 18kg of guarana extract (CAF 10%) are added, after stirring and dissolution, the temperature is kept at 60 ℃ for 1 hour, 10kg of L-carnitine and 100kg of xylitol dry powder are added, after stirring and dissolution, filtration is carried out, after reduced pressure concentration, spray drying is carried out, and about 360kg of composition dry powder is obtained.
Taking 200kg of composition dry powder, adding appropriate amount of composite VB and VC dry powder, mixing and blending uniformly, and quantitatively subpackaging 20 g/bag to obtain the dihydromyricetin solid beverage.
Specification and content: 20 g/bag; DMY content about 25mg/g, CAF about 5mg/g, gamma-CD about 130mg/g, pH about 3.9.
Example 6:
dihydromyricetin tea beverage
Preparation of 1% vine tea, black tea and lemon extract: mixing 20kg of vine tea, 25kg of black tea and 30kg of dried lemon with 1000kg of purified water, heating to 90 ℃ under stirring, keeping the temperature for 30 minutes, filtering and collecting filtrate, adding water into filter residue, repeatedly extracting for 1 time, combining the filtrate, adding 0.05% of pectinase, keeping the temperature at 50 ℃ and stirring for 2 hours, then heating to 90 ℃ and keeping the temperature for 10 minutes, cooling, centrifuging (or filtering/ultrafiltering) to obtain supernatant, and supplementing water to a constant volume of 2000L (kg), wherein the volume is 1% of the vine tea, black tea and lemon extract.
2000kg of 1% vine tea black tea lemon extract is taken, 20kg of gamma-CD and 100kg of RS are added, stirring is carried out to dissolve the extract, then the heat preservation is carried out for 60 minutes at 50 ℃, then 1kg of vitamin C, taurine, stevioside and 2kg of xanthan gum are added, stirring and heating are carried out to 90 ℃, the dissolution is carried out for 10 minutes, a proper amount of sodium citrate is added, the pH value is adjusted to 3.5, 200 meshes of filtration is carried out, filtrate is collected, the filtrate is rapidly cooled to 92 ℃ after UHT ultrahigh temperature instant sterilization (125 ℃ x 3-8 seconds), sterile hot filling is carried out for 200 ml/bottle (tank), the bottle is inverted for 50 seconds, then spray cooling is carried out to about 40 ℃, drying, labeling and inspection are carried out.
Specification and content: 200 ml/bottle (can); DMY content of about 3mg/g, CAF content of about 0.3mg/g, gamma-CD of about 10mg/g, RS content of about 50mg/g, pH of about 3.5.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the scope of the invention, which is defined by the claims appended hereto, and any other technical entity or method that is encompassed by the claims as broadly defined herein, or equivalent variations thereof, is contemplated as being encompassed by the claims.
Claims (8)
1. The invention provides a composition rich in dihydromyricetin, which is characterized by being selected from one of the following two conditions:
1) dihydromyricetin-caffeine-resistant dextrin (DMY-CAF-RS) composition, wherein the DMY content is more than or equal to 1.0mg/g, the CAF content is more than or equal to 0.050mg/g, the content ratio of DMY to CAF (DMY/CAF) is 0.30-30, and the RS content is more than or equal to 1.0 mg/g; preferably, DMY is more than or equal to 2.0mg/g, CAF is more than or equal to 0.10mg/g, wherein DMY/CAF is 0.60-20, and RS is more than or equal to 3.0 mg/g; more preferably, DMY is more than or equal to 3.0mg/g, CAF concentration is more than or equal to 0.20mg/g, DMY/CAF is 1-15, and RS is more than or equal to 5.0 mg/g.
2) Dihydromyricetin-caffeine-cyclodextrin (DMY-CAF-CD) composition, wherein DMY content is not less than 1.0mg/g, CAF is not less than 0.050mg/g, DMY/CAF is 0.30-30, and CD is not less than 0.50 mg/g; preferably, the concentration of DMY is more than or equal to 2.0mg/g, the concentration of CAF is more than or equal to 0.10mg/g, the concentration of DMY/CAF is 0.60-20, and the concentration of CD is more than or equal to 1.0 mg/g; more preferably, DMY is not less than 3.0mg/g, CAF is not less than 0.20mg/g, DMY/CAF is 1-15, and CD is not less than 1.5 mg/g.
2. The composition of claim 1, wherein the cyclodextrin comprises α -cyclodextrin, β -cyclodextrin, γ -cyclodextrin, and derivatives thereof.
3. The composition of claim 1, wherein the source of DMY comprises Ampelopsis grossedentata, Ampelopsis grossedentata extract, and DMY-rich food or medicinal materials and extracts thereof.
4. The composition of claim 1, wherein the source of CAF includes, but is not limited to: guarana extract, tea extract (including black tea, oolong tea, green tea, white tea, etc.), caffeine synthetic product and their compound products.
5. The composition of claim 1, wherein the optional pH is 7.0 or less when the product attribute is liquid; the pH is preferably less than or equal to 6.0; more preferably, the pH is less than or equal to 5.0.
6. The composition of claim 1, wherein the composition of the present invention comprises, in addition to DMY, CAF, RS (and/or CD), a food or pharmaceutical acceptable carrier, including but not limited to (1) liquids such as water, saline, glycerol, ethanol and alcoholic beverages containing ethanol, (2) adjunct ingredients such as emulsifiers, pH buffering substances, alginate gels, pectin, sodium carboxymethylcellulose (CMC), xanthan gum, gellan gum, guar gum, carrageenan, citric acid, sodium citrate, malic acid, sodium malate, sucrose, fructose, maltitol, steviol glycosides and the like, (3) nutrients such as L-carnitine, taurine, arginine, soluble proteins (peptides), vitamin B, vitamin C, vitamin E, β -carotene, calcium, zinc, selenium and the like, (4) single or compound extracts from plants and (or) herbs, fruit and vegetable juices and the like.
7. The composition of claim 1, wherein the product form comprises: (1) liquid products including oral liquids, beverages, suspensions, gels and creams; (2) solid products including powders, granules, capsules and tablets.
8. A process for the preparation of a composition according to claim 1, characterized in that the process steps are selected from the following:
1) extracting to obtain DMY extract, wherein the DMY extract comprises DMY pure product (content is more than or equal to 98%) extracted from vine tea and other raw materials and extract with lower DMY content; and can also be purchased commercially.
2) Extracting to obtain CAF extract, including CAF pure product and crude extract extracted from CAF-rich raw material, guarana extract, and tea extract with various CAF contents; and can also be purchased commercially.
3) Mixing to obtain DMY-CAF-RS/CD composition, wherein: mixing DMY extract, CAF extract and RS (or CD) according to the composition proportion of the composition, adding proper amount of carrier if necessary, stirring and dissolving to form a complex. Preferably, the method comprises dissolving the compound at a temperature above 30 ℃ for at least 10 minutes, more preferably at a temperature of 40-95 ℃ for at least 15 minutes.
4) The product blending is characterized in that: adding a proper amount of the carrier of the invention into the composition, heating, dissolving and blending to obtain the required concentration and volume; adding a proper amount of acid or alkali to adjust the pH value to the required value, and is characterized in that the pH value is selected to be less than or equal to 7.0, wherein the pH value is preferably less than or equal to 6.0, and the pH value is more preferably less than or equal to 5.0.
5) Centrifuging or filtering the product concoction solution to remove insoluble particles, collecting clarified solution (or filtrate), and bottling according to set volume, and performing pasteurization (such as water bath at 90 deg.C for 15 min) or pre-sterilization (such as ultra-high temperature instantaneous sterilization UHT/125 deg.C for 3-8 s), and hot-filling or aseptic canning to obtain beverage.
6) For preparing solid products, after obtaining the DMY-CAF-RS/CD composition, the clear liquid (or filtrate) is collected by centrifugation (or filtration), concentrated and dried into dry powder or particles, and then prepared into powder or granules packaged quantitatively, or prepared into capsules or tablets.
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| CN111543636A (en) * | 2020-06-03 | 2020-08-18 | 王京杭 | Flavone high-fiber composition and preparation method thereof |
| CN112451514A (en) * | 2020-11-26 | 2021-03-09 | 江西农业大学 | Dihydromyricetin nano-selenium and preparation method and application thereof |
| CN112715939A (en) * | 2020-12-30 | 2021-04-30 | 杭州娃哈哈科技有限公司 | Preparation method of dihydromyricetin compound solution capable of being stably stored for long time |
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| US20050084574A1 (en) * | 2003-09-12 | 2005-04-21 | Kao Corporation | Preparation process of tea extract |
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| US20050084574A1 (en) * | 2003-09-12 | 2005-04-21 | Kao Corporation | Preparation process of tea extract |
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Cited By (4)
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| CN111543636A (en) * | 2020-06-03 | 2020-08-18 | 王京杭 | Flavone high-fiber composition and preparation method thereof |
| CN112451514A (en) * | 2020-11-26 | 2021-03-09 | 江西农业大学 | Dihydromyricetin nano-selenium and preparation method and application thereof |
| CN112715939A (en) * | 2020-12-30 | 2021-04-30 | 杭州娃哈哈科技有限公司 | Preparation method of dihydromyricetin compound solution capable of being stably stored for long time |
| CN112715939B (en) * | 2020-12-30 | 2023-03-10 | 杭州娃哈哈科技有限公司 | Preparation method of dihydromyricetin compound solution capable of being stably stored for long time |
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