CN112741237A - Concentrated fruit juice capable of keeping stable content of astragaloside and preparation method thereof - Google Patents

Concentrated fruit juice capable of keeping stable content of astragaloside and preparation method thereof Download PDF

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Publication number
CN112741237A
CN112741237A CN202110081126.6A CN202110081126A CN112741237A CN 112741237 A CN112741237 A CN 112741237A CN 202110081126 A CN202110081126 A CN 202110081126A CN 112741237 A CN112741237 A CN 112741237A
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astragalus
astragaloside
extract
solution
water
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张连富
魏孔炯
徐琳
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Gansu Yucuitang Nutrition Health Food Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/385Concentrates of non-alcoholic beverages
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52Adding ingredients
    • 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
    • A23L2/52Adding ingredients
    • A23L2/60Sweeteners
    • 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
    • A23L2/52Adding ingredients
    • A23L2/68Acidifying substances
    • 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
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/17Amino acids, peptides or proteins
    • A23L33/175Amino acids
    • 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

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Abstract

The invention discloses a concentrated fruit juice for keeping stable content of astragaloside and a preparation method thereof. The preparation method comprises the following steps: cutting astragalus into small pieces, soaking the small pieces in an alcohol-water solution containing edible ethanol, and filtering to obtain an extracting solution; step two, concentrating the extracting solution in vacuum until the solid content reaches 45-50%, and then adjusting the solid content of the extracting solution to 35-45% by using an acidity regulator solution, wherein the pH value of the extracting solution is more than or equal to 7, so as to obtain astragalus extract; step three, preparing concentrated juice with solid content of 15-20% by taking astragalus extract, initial concentrated juice and powdery water-soluble ingredients as main materials, and adjusting the pH value of the system to 4-5 by using an acidity regulator; and step four, fully and uniformly mixing the concentrated juice treated in the step three, filling the mixture into a bottle or a bag, and sterilizing to obtain a final product. The concentrated juice prepared by the invention has stable content of astragaloside IV in the whole storage period of the product and high nutritive value.

Description

Concentrated fruit juice capable of keeping stable content of astragaloside and preparation method thereof
Technical Field
The invention belongs to the technical field of traditional food functionalization, and particularly relates to a concentrated fruit juice product taking astragalus root as a main raw material and taking astragaloside as a main functional component and a preparation method thereof.
Background
Astragalus membranaceus is the root of Astragalus membranaceus bge of Leguminosae, is traditionally considered to have the effects of benefiting vital qi, strengthening spleen and stomach, expelling pus, relieving pain and activating blood, and generally needs to be effective in a certain dosage and long-term use. Modern pharmacological studies show that astragalus has remarkable effects of resisting fatigue, resisting inflammation, regulating immunity and the like, and the main functional components of the astragalus comprise flavonoids, saponins, saccharides, organic acids, amino acids and the like, wherein the astragalus saponin IV, namely the astragaloside IV has the most remarkable effect.
With the continuous and high-speed development of various careers of the economic society of China and the continuous improvement of the living standard of people, the demand of the whole society on safe and healthy diet is continuously increased. Based on the cognition of the traditional medicine on the beneficial health effect of the astragalus and the continuous progress of the modern processing technology, various functional foods and Chinese medicinal preparations taking the astragalus as the main raw material are continuously emerged, and a large number of patents are formed, such as a compound astragalus Chinese medicinal preparation (publication number: CN101284041B, publication number: 2010.12.22) with the effects of resisting fatigue and anoxia, a health drink (publication number: CN1397220A, publication number: 2003.02.19) containing the components of the natural plant astragalus and cassia bark, the application of the astragalus extract in the preparation of the anti-fatigue medicine (publication number: CN1772036A, publication number: 2006.05.17), the preparation method of the astragalus health drink (publication number: CN101530230A, publication number: 2009.09.16), the astragalus health food and the preparation method thereof (publication number: CN101849630A, publication number: 2010.10.06), an astragalus polysaccharide and lycium polysaccharide composition and the preparation method and the application thereof (publication number: CN103609939A, publication number: 2014.03.05), Astragalus mongholicus and medlar health-preserving traditional Chinese medicine tea beverage and preparation method (publication number: CN104322729A, publication number: 2015.02.04), ginseng and astragalus mongholicus health-preserving traditional Chinese medicine tea beverage and preparation method (publication number: CN104304536A, publication number: 2015.01.28), astragalus mongholicus qi-tonifying and exterior-consolidating health-care beverage and production method thereof (publication number: CN105687976A, publication number: 2016.06.22), anti-fatigue health-care food containing astragalus mongholicus, eucommia ulmoides, polygonatum sibiricum, sea buckthorn and ginseng and preparation method thereof (publication number: CN104489647A, publication number: 2015.04.08), astragalus mongholicus compound anti-fatigue beverage and preparation method thereof (publication number: CN105851748A, publication number: 2016.08.17), antioxidant anti-fatigue astragalus mongholicus functional beverage and preparation process thereof (publication number: CN106107340A, publication number: 2016.11.16), astragalus mongholicus and medlar compound beverage and preparation method thereof (publication number: CN110495544A, publication number: 2019.11.26), astragalus mongholicus compound anti-fatigue beverage and preparation method thereof (publication number: CN108991307A, publication number: 2018.12.14), A health food containing fructus Lycii and radix astragali and its preparation method (publication No. CN109315774A, published as 2019.02.12), and preparation method of antifatigue composition containing radix astragali as main material (publication No. CN109393283A, published as 2019.03.01) are provided. However, in general, the function claims are mainly focused on fatigue resistance, and innovation points are mainly focused on raw material combination screening, most of the raw materials are the combination of astragalus, medlar (lycium barbarum polysaccharide), ginseng, polygonatum sibiricum, even sea buckthorn, eucommia ulmoides, cinnamon and the like, and the product forms mainly comprise powder, beverage, oral liquid and the like. The above-mentioned patent applications have common drawbacks: 1. the content of the main active ingredient astragaloside in the product, particularly the stability of the astragaloside in the whole product period is not concerned, but a widely accepted fact is that (i) the water solubility of the astragaloside is poor, the solubility of the astragaloside in an aqueous phase is only 0.05mg/mL at 20 ℃, and the excess astragaloside is easy to separate out from the system and cannot be utilized, as described in patent CN108498457A (published: 2018.09.07); ② mutual transformation between astragalosides I and II and astragaloside IV can be promoted under different pH conditions (Yuandan Zhengmin, a method for quantifying common crude drugs in Japan-radix astragali, foreign medicine and botanical drug Manual, 1990, Vol 5, No 5, P201-2); CHU Chu, LIU E-Hu, QI Lian-Wen, LI Ping, Chinese Journal of Natural medicinal herbs, 2014,12(4):314-20), astragaloside IV content is greatly influenced by system pH; 2. the influence of the processing technology, parameters and product environment (pH) on the stability of the astragaloside cannot be researched and optimized. The patent "a soluble astragaloside IV complex with high stability and its preparation method" (CN108498457A) describes a soluble astragaloside IV complex, but it needs to be coated by rebaudioside A and glycyrrhizic acid, and its form is micelle, and can not be compounded with other functional components (raw materials), so its application is limited. An astragalus and pear juice composition, an astragalus and pear juice beverage prepared from the same and a preparation method thereof (publication number: CN109452502A, published Japanese 2019.03.12), an astragalus and blueberry composition, an astragalus and blueberry beverage prepared from the same and a preparation method thereof (publication number: CN109363009A, published Japanese 2019.02.22), an astragalus and blueberry composition, an astragalus and beverage prepared from the same and a preparation method thereof (publication number: CN109619329A, published Japanese 2019.04.16) respectively describe fruit and vegetable juice products containing astragalus raw materials, but the two problems are not researched.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides concentrated fruit juice capable of keeping the content of astragaloside stable and a preparation method thereof. The concentrated fruit juice is prepared by taking astragalus root as a main raw material, taking astragaloside as a main effective component, compounding a Chinese date extract, a ginseng extract, a guanala extract, sorbitol, xylitol, xanthan gum, concentrated apple juice, an acidity regulator and the like, and realizes the stability of the astragaloside content in the product in the whole product period.
In order to achieve the purpose, the invention adopts the following technical scheme:
a concentrated fruit juice for keeping stable content of astragaloside is prepared by the following preparation method:
cutting astragalus into small pieces, soaking the small pieces in an alcohol-water solution containing edible ethanol, and filtering to obtain an extracting solution;
step two, concentrating the extracting solution in vacuum until the solid content reaches 45-50%, and then adjusting the solid content of the extracting solution to 35-45% by using an acidity regulator solution, wherein the pH value of the extracting solution is more than or equal to 7, so as to obtain astragalus extract;
step three, preparing concentrated juice with solid content of 15-20% by taking astragalus extract, initial concentrated juice and powdery water-soluble ingredients as main materials, and adjusting the pH value of the system to 4-5 by using an acidity regulator;
and step four, fully and uniformly mixing the concentrated juice treated in the step three, filling the mixture into a bottle or a bag, and sterilizing to obtain a final product.
As an improved technical scheme of the invention, in the first step, the astragalus is astragalus root hairs with the water content of less than 10 percent, and is cut into particles with the length of less than 3 mm; the alcohol-water solution is prepared by adding edible ethanol into purified water, the volume ratio of the ethanol to the purified water is 15-25%, the soaking time is 6-12 h, and the mass of astragalus membranaceus soaked in each liter of the alcohol-water solution is 0.4-0.6 kg.
As a further improved technical scheme, in the first step, the volume ratio of ethanol to purified water in the alcohol-water solution is 19-21%, and the soaking time is 8-10 hours.
And (2) as an improved technical scheme of the invention, soaking the filter residue filtered in the step one in an alcohol-water solution containing edible ethanol, continuing to soak and extract, then filtering to obtain an extracting solution II, and mixing the extracting solution II with the extracting solution obtained in the step one for use in the step two.
As an improved technical scheme of the invention, in the first step, the filtration is finished by two times, wherein the first time is the filtration by a 20-40 mesh filter screen, and the second time is the filtration by a 100-200 mesh filter screen.
As an improved technical scheme of the invention, in the second step, the vacuum concentration process parameters are that the vacuum degree is 0.05-0.1MPa, and the temperature of the feed liquid is 45-65 ℃. Preferably, the vacuum degree is 0.08Mpa, and the temperature of the feed liquid is 50-60 ℃.
In the second and third steps, the acidity regulator comprises one or a mixture of monosodium fumarate, tricalcium phosphate, calcium hydrogen phosphate, calcium dihydrogen phosphate, tripotassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, trisodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium citrate, potassium hydrogen citrate, potassium dihydrogen citrate, trisodium citrate, sodium hydrogen citrate and sodium dihydrogen citrate.
As an improved technical scheme of the invention, in the third step, the solid content of the initial concentrated fruit juice is 30-70%, and the ingredients comprise one or a mixture of a nutrition enhancer, a plant extract, a low-heat sweetener and a thickening agent.
As a further improved technical scheme of the invention, the initial concentrated juice comprises one or a mixture of apple, peach, medlar and jujube concentrated juice.
As a further improved technical scheme of the invention, the nutrition enhancer comprises one or a mixture of theanine, gamma-aminobutyric acid and taurine.
As a further improved technical scheme of the invention, the plant extract comprises one or a mixture of ginseng extract, guarana extract, green tea extract and eucommia bark extract.
As a further improved technical scheme of the invention, the low-calorie sweetener comprises one or a mixture of xylitol, sorbitol, fructo-oligosaccharide, isomalto-oligosaccharide and xylo-oligosaccharide.
As a further improved technical scheme of the invention, the thickening agent comprises one or a mixture of xanthan gum, pectin and modified starch.
As an improved technical scheme of the invention, the mixing and homogenizing process in the step four is completed by using a colloid mill.
As an improved technical scheme of the invention, the sterilization process comprises the steps of heating at a high temperature of 90-100 ℃ for 20-40min, and then cooling. Preferably, the sterilization process is heating at a high temperature of 95 ℃ for 30min, and then cooling.
The invention also provides a preparation method for preparing the concentrated fruit juice keeping the astragaloside content stable.
Has the advantages that:
the invention selects dry (the water content is less than 10%) radix astragali root hair as raw material, cuts into pieces with the length less than 3mm, takes alcohol-water solution with edible alcohol accounting for 15-25% (V/V) as extracting agent, according to the proportion of 1: 2 (the mass of the root hairs of the astragalus/the volume of the extracting agent) is soaked for 6 to 12 hours at room temperature, 20 percent alcohol-water solution with the volume being 1 time that of the filter residues is added, the soaking and the stirring are continued for 30 minutes at room temperature, the two filtrates are filtered by a filter screen with 20 to 40 meshes to separate the broken residues of the astragalus, then the two filtrates are combined and filtered by a filter screen with 100 meshes and 200 meshes to obtain the extracting solution. Vacuum concentrating the extractive solution (vacuum degree of 0.05-0.1MPa, material liquid temperature of 45-65 deg.C) until solid content reaches 45-50%, and adjusting solid content of the extractive solution to 35-45% with acidity regulator solution, and pH not less than 7 to obtain radix astragali extract. Therefore, the astragalus extract with the content of the astragaloside reaching 0.81-0.90mg/g can be prepared in a relatively short time (usually 15h), the extraction efficiency of the raw material astragalus is improved, the stability of the astragaloside in the extract is realized, and the subsequent preparation of concentrated juice is convenient. On the basis, the astragalus extract is used as a base, concentrated fruit juice (the solid content is 30-70 percent), a nutrition enhancer, a plant extract, a low-heat sweetener, a thickening agent and an acidity regulator are prepared, the solid content of the product is controlled to be 15-20 percent (W/W), the pH value of the product is adjusted to be 4-5 by using an acidity regulator solution, and the product is prepared after full mixing, filling and sterilization. The combination of high solid content (15-20%), pH value (pH4-5) of acidic food and sterilization conditions (95 ℃ and 30min) is accurately controlled to realize the whole-period content stability of astragaloside IV in the product and the biological safety of the product.
Drawings
FIG. 1 is a liquid chromatogram of a standard astragaloside IV sample;
FIG. 2 is a liquid chromatogram of the product of example 1.
Detailed Description
The invention will now be described in detail with reference to specific embodiments and drawings for the purpose of providing a clear understanding of the invention to those skilled in the art.
Example 1
1. Pretreatment and extraction of astragalus membranaceus raw material
1) Selecting raw materials: cutting dried radix astragali root hair (water content less than 10%) into pieces with length less than 3 mm;
2) preparing a solvent: adding edible ethanol into purified water to obtain ethanol water solution with ethanol content of 20% (V/V) as extractant;
3)5 kg of astragalus root crushed aggregates are added into 10L of 20 percent edible ethanol and soaked for 8 hours at the room temperature of 20 ℃;
4) pouring out the liquid in the extraction container and sieving the liquid by a 40-mesh filter screen to obtain an extracting solution I;
5) placing the residue of radix astragali obtained in 4) into extraction container, adding 5L 20% edible ethanol solution again, and extracting at room temperature under low speed stirring for 30 min;
6) separating the liquid in the step 5) (filtering residues are properly squeezed to discharge residual liquid) and sieving the liquid through a 40-mesh filter screen to obtain an extracting solution II;
7) mixing the extractive solutions I and II, and filtering with 200 mesh filter screen to remove fine particles.
2. Treatment of the extract
Filtering the extractive solution, vacuum concentrating (vacuum degree of 0.08MPa, feed liquid temperature of 50) deg.C until solid content reaches 47%, and adjusting solid content of the extractive solution to 40% and pH of 9.0 with acidity regulator (trisodium phosphate) solution to obtain radix astragali extract.
3. Preparation of concentrated fruit juice
1) Packing 1000 small packages each time, each small package (bag/bottle) has a volume of 30mL, and the dosage of the astragalus extract is 2.12g calculated by 1.80mg of astragaloside;
2) ingredient selection and addition amount:
Figure BDA0002909352180000061
3) preparation of
Mixing the selected acidity regulator (monosodium fumarate) with warm water, stirring to dissolve, and preparing into 5% solution;
mixing the selected thickener with low calorie sweetener, and pre-dissolving in warm water (30 deg.C) as little as possible;
adding other water soluble components including plant extract and nutrition enhancer into warm water (30) deg.C as little as possible respectively for pre-dissolving;
quantitatively mixing radix astragali extract, concentrated fruit juice, thickener aqueous solution, plant extract aqueous solution and nutrition enhancer aqueous solution, primarily mixing, adding water to approximate 29.5L, adjusting pH to 4.55 with acidity regulator solution, and controlling total solid content of the solution at 16% (W/W);
4) finally adding water to a constant volume to be scaled (30L) and stirring uniformly;
5) the further dispersion was treated with a colloid mill and the concentrated juice had a density of about 1.1g/mL after dispersion.
4. Packaging and sterilization
1) And (3) metering and packaging according to standard volume: 30-50 mL;
2) and (3) sterilization: on the premise of meeting the requirement of killing microorganisms, selecting sterilization conditions with the minimum influence on taste and the like; sterilizing at 95 deg.C for 30min, and cooling.
5. Determination of astragaloside
1) Sensory evaluation;
2) liquid chromatography analysis: taking about 4g of astragalus mongholicus traditional Chinese medicine powder, precisely weighing, placing in a Soxhlet extractor, adding 40mL of methanol, cold soaking overnight, adding an appropriate amount of methanol, heating and refluxing for 4 hours, recovering a solvent from an extracting solution, concentrating to dryness, adding 10mL of water into residue, slightly heating to dissolve the residue, shaking and extracting for 4 times by using water-saturated n-butyl alcohol, 40mL each time, combining n-butyl alcohol solutions, fully washing for 2 times by using an ammonia test solution, 40mL each time, discarding the ammonia solution, evaporating the n-butyl alcohol solution to dryness, adding 5mL of water into the residue to dissolve the residue, cooling, passing through a D101 type macroporous adsorption resin column (the inner diameter is 1.5cm, the column height is 12cm), eluting with 50mL of water, discarding an aqueous solution, eluting with 30mL of 40% ethanol, discarding an eluent, then eluting with 80mL of 70% ethanol, collecting the eluent, evaporating to dryness, dissolving the residue with methanol, transferring to a 5mL volumetric flask. Precisely sucking 20 microliters of control solution and 20 microliters of test solution, respectively, and injecting into a liquid chromatograph (chromatographic conditions: chromatographic column C18 (150mm × 4.6mm,3.5 μm), mobile phase acetonitrile-water (35: 65), flow rate of 1 mL/min-1(ii) a The column temperature is 30; air flow rate of ELSD detectorDegree 2.5 L.min-1And measuring the temperature of the drift tube at 110) DEG C, and calculating by using an external standard two-point method logarithmic equation to obtain the drift tube.
6. Test results
Sensory evaluation results: color 5 points, clarity 4 points, smell 4 points, taste 5 points, and total score 18 points.
The test results are shown in fig. 1 and 2. FIG. 1 is a liquid chromatogram of a standard astragaloside IV sample; FIG. 2 is a liquid chromatogram of the product of this example as prepared.
According to the test, the content of the astragaloside in the astragalus extractum in the step 2 is 0.85 +/-0.03 mg/g, and after the astragalus extractum is prepared into concentrated juice, the content of the astragaloside in the product is 6 +/-0.15 mg/100 mL. After the product is stored for 18 months at room temperature, the content of the astragaloside in the product is 5.6 +/-0.04 mg/100mL, and the retention rate is as high as 93.3%.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000081
example 2
1. Pretreatment and extraction of astragalus membranaceus raw material
1) Selecting raw materials: cutting dried radix astragali root hair (water content less than 10%) into pieces with length less than 3 mm;
2) preparing a solvent: adding edible ethanol into purified water to obtain ethanol water solution with ethanol content of 20% (V/V) as extractant;
3)5 kg of astragalus root crushed aggregates are added into 10L of 20 percent edible ethanol and soaked for 10 hours at the room temperature of 25 ℃;
4) pouring out the liquid in the extraction container and sieving the liquid by a 20-mesh filter screen to obtain an extracting solution I;
5) placing the residue of radix astragali obtained in 4) into extraction container, adding 5L 20% edible ethanol solution again, and extracting at room temperature under low speed stirring for 30 min;
6) separating the liquid in the step 5) (filtering residues are properly squeezed to discharge residual liquid) and sieving the liquid through a 40-mesh filter screen to obtain an extracting solution II;
7) mixing the extractive solutions I and II, and filtering with 100 mesh filter screen to remove fine particles.
2. Treatment of the extract
Filtering the extractive solution, vacuum concentrating (vacuum degree of 0.08MPa, feed liquid temperature of 55 deg.C) until solid content reaches 50%, and adjusting solid content of the extractive solution to 40% and pH 9.5 with acidity regulator (trisodium citrate) solution to obtain radix astragali extract.
3. Preparation of concentrated fruit juice
1) Packing 1000 small packages each time, each small package (bag/bottle) has a volume of 30mL, and the dosage of the astragalus extract is 2.05g calculated by 1.80mg of astragaloside;
2) ingredient selection and addition amount:
Figure BDA0002909352180000082
Figure BDA0002909352180000091
3) preparation of
Mixing the selected acidity regulator (sodium dihydrogen citrate, sodium hydrogen citrate) with warm water, stirring to dissolve, and making into 5% solution;
mixing the selected thickener with low calorie sweetener, and pre-dissolving in warm water (35 deg.C) as little as possible;
adding other water soluble components including plant extract and nutrition enhancer into warm water (35) deg.C as little as possible respectively for pre-dissolving;
quantitatively mixing radix astragali extract, concentrated fruit juice, thickener aqueous solution, plant extract aqueous solution and nutrition enhancer aqueous solution, primarily mixing, adding water to approximate 29.5L, adjusting pH to 4.6 with acidity regulator solution, and controlling total solid content of the solution at 17% (W/W);
4) finally adding water to a constant volume to be scaled (30L) and stirring uniformly;
5) the further dispersion was treated with a colloid mill to obtain a concentrated juice having a density of about 1.1 g/mL.
4. Packaging and sterilization
1) And (3) metering and packaging according to standard volume: 30-50mL
2) And (3) sterilization: on the premise of meeting the requirement of killing microorganisms, selecting sterilization conditions with the minimum influence on taste and the like; sterilizing at 95 deg.C for 30min, and cooling.
5. Test results
Sensory evaluation results: color 5 points, clarity 4 points, smell 5 points, taste 5 points, and total score 19 points.
Liquid chromatography test results: the content of the astragaloside in the astragalus extractum in the step 2 is 0.88 +/-0.10 mg/g. Storing at room temperature for 18 months, the retention rate of astragaloside in the product is 91.8%.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000092
example 3
1. Pretreatment and extraction of astragalus membranaceus raw material
1) Selecting raw materials: cutting dried radix astragali root hair (water content less than 10%) into pieces with length less than 3 mm;
2) preparing a solvent: adding edible ethanol into purified water to obtain ethanol water solution with ethanol content of 20% (V/V) as extractant;
3)5 kg of astragalus root crushed aggregates are added into 10L of 20 percent edible ethanol and soaked for 9 hours at room temperature (25) DEG C;
4) pouring out the liquid in the extraction container and sieving the liquid by a 20-mesh filter screen to obtain an extracting solution I;
5) placing the residue of radix astragali obtained in 4) into extraction container, adding 5L 20% edible ethanol solution again, and extracting at room temperature under low speed stirring for 30 min;
6) separating the liquid in the step 5) (filtering residues are properly squeezed to discharge residual liquid) and sieving the liquid through a 20-mesh filter screen to obtain an extracting solution II;
7) mixing the extractive solutions I and II, and filtering with 200 mesh filter screen to remove fine particles.
2. Treatment of the extract
Vacuum concentrating the filtrate (vacuum degree of 0.08MPa, feed liquid temperature of 60) deg.C until solid content reaches 50%, and adjusting solid content of the extract to 40% with acidity regulator solution (potassium dihydrogen phosphate, potassium hydrogen phosphate) and pH of 7.5.
3. Preparation of concentrated fruit juice
1) Packing 1000 small packages each time, each small package (bag/bottle) has a volume of 30mL, and calculating the dosage of the radix astragali extract to be 2.22g according to the content of 1.80 +/-0.02 mg of astragaloside;
2) ingredient selection and addition amount:
Figure BDA0002909352180000101
3) preparation of
Mixing the selected acidity regulators (potassium dihydrogen phosphate and potassium hydrogen phosphate) with warm water, stirring until the acidity regulators are dissolved, and preparing a solution with the concentration of 5% for later use;
mixing the selected thickener with low calorie sweetener, and pre-dissolving in warm water (40) deg.C as little as possible;
adding other water soluble components including plant extract and nutrition enhancer into warm water (40) deg.C as little as possible respectively for pre-dissolving;
quantitatively mixing radix astragali extract, concentrated fruit juice, thickener aqueous solution, plant extract aqueous solution and nutrition enhancer aqueous solution, primarily mixing, adding water to approximate 29.5L, adjusting pH to 4.65 with acidity regulator solution, and controlling total solid content of the solution at 18% (W/W);
4) finally adding water to a constant volume to be scaled (30L) and stirring uniformly;
5) the further dispersion was treated with a colloid mill to give a concentrated juice density of about 1.1g/mL after dispersion.
4. Packaging and sterilization
1) And (3) metering and packaging according to standard volume: 30-50mL
2) And (3) sterilization: on the premise of meeting the requirement of killing microorganisms, selecting sterilization conditions with the minimum influence on taste and the like; sterilizing at 95 deg.C for 30min, and cooling.
5. Test results
Sensory evaluation results: : color 5 points, clarity 4 points, smell 5 points, taste 4 points, and total score 18.
Liquid chromatography test results: the content of the astragaloside in the astragalus extractum in the step 2 is 0.81 +/-0.02 mg/g. Storing at room temperature for 18 months, the retention rate of astragaloside in the product is 90.2%.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000111
example 4
The present embodiment is different from embodiment 1 in that: in step 4, the sterilization temperature is 100 ℃ and the sterilization time is 20 min.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000112
example 5
The present embodiment is different from embodiment 1 in that: in step 4, the sterilization temperature is 90 ℃ and the sterilization time is 40 min.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000121
example 6
The present embodiment is different from embodiment 1 in that: in the step 3, the total solid content of the solution is controlled to be 15% (W/W), the addition amount of the concentrated peach juice (containing the solid content of 65%) is 0.65g, and the addition amounts of other substances are unchanged.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000122
example 7
The present embodiment is different from embodiment 1 in that: in the step 3, the total solid content of the solution is controlled to be 20% (W/W), the addition amount of the concentrated peach juice (containing 65% of the solid content) is 3.18g, and the addition amount of other substances is not changed.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000123
example 8
The present embodiment is different from embodiment 1 in that: in step 3, the pH value is adjusted to 4 by using an acidity regulator solution.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000124
example 9
The present embodiment is different from embodiment 1 in that: in step 3, the pH value is adjusted to 5 by using an acidity regulator solution.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000131
example 10
The present embodiment is different from embodiment 1 in that: in step 3, the pH value is adjusted to 7.9 by using an acidity regulator solution (sodium dihydrogen citrate and trisodium phosphate).
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000132
example 11
The present embodiment is different from embodiment 1 in that: in the step 2, the step of adjusting the astragalus extract to be alkaline is omitted. And (3) determining the content of the astragaloside in the astragalus extractum in the step (2) to be 0.46 +/-0.03 mg/g. In the step 3, 1000 small packages are still packed each time, the capacity of each small package (bag/bottle) is 30mL, the dosage of the astragalus extract is 3.91g calculated by 1.80mg of astragaloside, the addition amount of the concentrated peach juice (containing 65 percent of solid) is 0.05g, and the addition amounts of other substances are not changed.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000133
example 12
The present embodiment is different from embodiment 1 in that: in step 2, after the treatment of the alkaline step, the solid content in the astragalus extract is controlled to be 35%. The content of astragaloside in the astragalus extractum is measured to be 0.74 +/-0.02 mg/g. In the step 3, the astragalus extract is still packaged by 1000 small packages each time, the volume of each small package (bag/bottle) is 30mL, the dosage of the astragalus extract is 2.43g calculated by 1.80mg of the astragaloside, and the addition amount of other substances is unchanged.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000141
example 13
The present embodiment is different from embodiment 1 in that: in step 2, after the treatment of the alkaline step, the solid content in the astragalus extract is controlled to be 45%. The content of astragaloside in the astragalus extract is measured to be 0.86 +/-0.02 mg/g. In the step 3, the astragalus extract is packaged for 1000 small packages each time, the capacity of each small package (bag/bottle) is 30mL, the dosage of the astragalus extract is 2.09g calculated by 1.80mg of astragaloside, the addition amount of the concentrated peach juice (containing 65 percent of solid matters) is 1.02g, and the addition amount of other substances is unchanged.
The astragaloside content during the whole period of product storage is shown in the following table:
Figure BDA0002909352180000142
example 14
The present embodiment is different from embodiment 1 in that: in the step 1, the volume ratio of ethanol to water in the alcohol-water solution is 15%, and the soaking time is 12 hours. The content of astragaloside in the astragalus extract is measured to be 0.85 plus or minus 0.02 mg/g.
Example 15
The present embodiment is different from embodiment 1 in that: in the step 1, the volume ratio of ethanol to water in the alcohol-water solution is 19%, and the soaking time is 6 hours. The content of astragaloside in the astragalus extractum is measured to be 0.84 +/-0.04 mg/g.
Example 16
The present embodiment is different from embodiment 1 in that: in the step 1, the volume ratio of ethanol to water in the alcohol-water solution is 21%, and the soaking time is 12 hours. The content of astragaloside in the astragalus extract is measured to be 0.85 +/-0.04 mg/g.
Example 17
The present embodiment is different from embodiment 1 in that: in the step 1, the volume ratio of ethanol to water in the alcohol-water solution is 25%, and the soaking time is 8 hours. The content of astragaloside in the astragalus extract is measured to be 0.85 +/-0.03 mg/g.
The research of the patent finds that the processing technology, parameters and product environment (pH) of the concentrated fruit juice have obvious influence on the stability of the astragaloside. If the beverage is directly prepared from the concentrated astragalus extract, the link of regulating the pH of the astragalus extract to be more than or equal to 7 is not adopted, the defects of low extraction rate of the astragaloside and large consumption of astragalus raw materials and the defect of poor stability of the astragaloside during the storage period of the product exist. In addition, the astragaloside has higher requirement on the pH value of the product environment, the storage stability is good in a weak acid environment, and the storage stability is poor in a weak alkaline environment.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. It is to be understood that those skilled in the art may conceive of equivalent variations and modifications without departing from the scope of the present invention, and that the scope of the present invention is not to be considered as the same as the scope of the present invention.

Claims (10)

1. A method for preparing concentrated fruit juice with stable astragaloside content comprises the following steps:
cutting astragalus into small pieces, soaking the small pieces in an alcohol-water solution containing edible ethanol, and filtering to obtain an extracting solution;
step two, concentrating the extracting solution in vacuum until the solid content reaches 45-50%, and then adjusting the solid content of the extracting solution to 35-45% by using an acidity regulator solution, wherein the pH value of the extracting solution is more than or equal to 7, so as to obtain astragalus extract;
step three, preparing concentrated juice with solid content of 15-20% by taking astragalus extract, initial concentrated juice and powdery water-soluble ingredients as main materials, and adjusting the pH value of the system to 4-5 by using an acidity regulator;
and step four, fully and uniformly mixing the concentrated juice treated in the step three, filling the mixture into a bottle or a bag, and sterilizing to obtain a final product.
2. The method of claim 1, wherein: in the first step, the astragalus root is the astragalus root hair with the water content of less than 10 percent, and is cut into pieces with the length of less than 3 mm; the alcohol-water solution is prepared by adding edible ethanol into purified water, the volume ratio of the ethanol to the purified water is 15-25%, and the soaking time is 6-12 h; preferably, the volume ratio of ethanol to purified water in the alcohol-water solution is 19-21%, and the soaking time is 8-10 h; the weight of the astragalus root soaked in each liter of alcohol-water solution is 0.4-0.6 kg.
3. The method of claim 1, wherein: and (3) soaking the filter residue filtered in the step one in an alcohol-water solution containing edible ethanol, continuing soaking and extracting, then filtering to obtain an extracting solution II, and mixing the extracting solution II with the extracting solution obtained in the step one for use in the step two.
4. The method of claim 1, wherein: in the first step, the filtration is completed in two times, wherein the first time is the filtration with a 20-40 mesh filter screen, and the second time is the filtration with a 100-200 mesh filter screen.
5. The method of claim 1, wherein: in the second step, the vacuum concentration process parameters are that the vacuum degree is 0.05-0.1MPa, and the temperature of the feed liquid is 45-65 ℃; preferably, the vacuum degree is 0.08Mpa, and the temperature of the feed liquid is 50-60 ℃.
6. The method of claim 1, wherein: in the second and third steps, the acidity regulator comprises one or a mixture of monosodium fumarate, tricalcium phosphate, calcium hydrogen phosphate, calcium dihydrogen phosphate, tripotassium phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, trisodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium citrate, potassium hydrogen citrate, potassium dihydrogen citrate, trisodium citrate, sodium hydrogen citrate, sodium dihydrogen citrate.
7. The method of claim 1, wherein: in the third step, the solid content of the initial concentrated fruit juice is 30-70%, and the ingredients comprise one or a mixture of a nutrition enhancer, a plant extract, a low-heat sweetener and a thickening agent.
8. The method of claim 7, wherein: the initial concentrated juice comprises one or mixture of concentrated juice of fructus Mali Pumilae, fructus Persicae, fructus Lycii, and fructus Jujubae; the nutrition enhancer comprises one or a mixture of theanine, gamma-aminobutyric acid and taurine; the plant extract comprises one or more of Ginseng radix extract, Guarana extract, green tea extract, and Eucommiae cortex extract; the low-calorie sweetener comprises one or a mixture of xylitol, sorbitol, fructo-oligosaccharide, isomalto-oligosaccharide and xylo-oligosaccharide; the thickening agent comprises one or a mixture of xanthan gum, pectin and modified starch.
9. The method of claim 1, wherein: in the fourth step, the sterilization process comprises the steps of heating at the high temperature of 90-100 ℃ for 20-40min, and then cooling; preferably, the sterilization process comprises heating at a high temperature of 95 ℃ for 30min, and then cooling; preferably, the mixing and homogenizing process is performed by using a colloid mill.
10. A concentrated fruit juice with stable astragaloside content, which is obtained by the preparation method according to any one of claims 1 to 9.
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