CN105919112B - Ginseng and fritillaria ussuriensis health food and preparation method and application thereof - Google Patents

Ginseng and fritillaria ussuriensis health food and preparation method and application thereof Download PDF

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CN105919112B
CN105919112B CN201610456359.9A CN201610456359A CN105919112B CN 105919112 B CN105919112 B CN 105919112B CN 201610456359 A CN201610456359 A CN 201610456359A CN 105919112 B CN105919112 B CN 105919112B
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ginseng
health food
extracting
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CN105919112A (en
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郭建鹏
敖宇涛
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Yanbian University
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Yanbian University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8966Fritillaria, e.g. checker lily or mission bells
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258Panax (ginseng)
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

Abstract

The invention relates to a health food and a preparation method and application thereof, the health food is prepared by using ginseng and fritillaria ussuriensis as main raw materials in a formula, has the function of boosting immunity, and belongs to the field of development, production and use of health foods. The raw materials of the health food composition comprise 1-4 parts of ginseng and 1-3 parts of fritillary bulb, and the prepared preparation is granules, capsules and tablets. The preparation is prepared by the following process: firstly, preparing raw materials; pulverizing Ginseng radix; extracting fritillary bulb; extracting the ginseng; fifthly, concentrating and drying; preparing a soft material; granulating and finishing granules; and (8) forming. Function evaluation experiments show that the health food preparation produced according to the invention has the function of enhancing immunity.

Description

Ginseng and fritillaria ussuriensis health food and preparation method and application thereof
Technical Field
The invention relates to a health food and a preparation method and application thereof, in particular to a health food prepared by using ginseng and fritillaria ussuriensis as main raw materials in a formula, which has the function of enhancing immunity and belongs to the field of development, production and use of health foods.
Background
The invention relates to a health food composition with the function of enhancing immunity and a preparation method thereof, which are developed by taking the theory of national medicine of Korean nationalities (Korean medicine for short) as guidance according to the regulation of a health food registration management method. The formula of the composition is scientifically designed by referring to proved formulas for clinically preventing and treating lung qi deficiency of taiyin people according to the theory of four elephants medicine in medicine and pharmacology and by taking the immune function enhancement as an evaluation index and screening raw materials suitable for being used as health food and the dosage thereof through modern pharmacological experiments.
Ginseng Radix (Ginseng Radix et Rhizoma) is a herbal plant of AraliaceaePanax ginsengC.A. Mey dried root and rhizome, sweet, slightly bitter and slightly warm in taste. It enters spleen, lung, heart and kidney meridians. Has effects of invigorating primordial qi, recovering pulse, relieving depletion, invigorating spleen, benefiting lung, promoting fluid production, nourishing blood, tranquilizing mind, and improving intelligence. Can be used for treating asthenia, collapse, cold limbs, weak pulse, spleen deficiency, anorexia, lung deficiency, cough, asthma, body fluid deficiency, thirst, internal heat, diabetes, deficiency of both qi and blood, asthenia, palpitation, insomnia, sexual impotence, and cold womb. The Ginseng radix contains various ginsenoside, volatile oil, peptide, amino acids, microelements, organic acid, saccharide, various vitamins, choline and enzyme. Wherein the saponins are the main active components of Ginseng radix. Ginseng has effects on nervous system, cardiovascular system, endocrine system, digestive system, and reproductive system of human or animalHas obvious effect.
The earliest existing pharmaceutical monograph in China lists ginseng as the top grade in Shen nong Ben Cao Jing, which means that the ginseng has the effects of tonifying five internal organs, calming the spirit, calming the soul, stopping palpitation, eliminating pathogenic factors, improving eyesight, developing heart and intelligence, losing weight and prolonging life after long-term use. "the efficacy of the drug. Ginseng plays a great role in the treatment of diseases from ancient times to present, and has numerous effective prescriptions, such as Shengmai powder, Sijunzi decoction, Dushen decoction, Buzhong Yiqi decoction, Shenling Baizhu powder and the like. With the development of science and technology, ginseng is researched more and more deeply. Modern medical research and clinical practice prove that ginseng contains various ginsenosides, polysaccharides, amino acids, volatile oil, enzymes of ginseng, vitamins and the like, has the effects of nourishing and strengthening the body and delaying senility, has obvious treatment effect on senile diseases, deficiency syndrome and low immunity, can regulate in-vivo metabolism, such as regulating blood sugar and blood fat, has the effect on coronary heart disease, heart failure and arrhythmia, and has the effects of enhancing the excitation and inhibition processes of higher nerve activity, improving the flexibility of the nerve activity process and enhancing the mental labor function (intelligence development). The ginseng plays an important role in disease treatment and has wide development space for modern health care.
Bulbus Fritillariae Ussuriensis (Fritillariae Ussuriensis Bulbus) belonging to LiliaceaeFritillaria ussuriensis Maxim dried bulb is collected in spring, removed of outer skin, fibrous root and silt, and dried in the sun or at low temperature. Pingbei mother is bitter, sweet and slightly cold in nature, and enters lung and heart meridians; has the functions of clearing heat, moistening lung, reducing phlegm, relieving cough and the like; can be used for treating lung heat dry cough, dry cough with little phlegm, cough due to yin deficiency with bloody phlegm. Mainly produced in the northeast province, and most of the commodities are cultivated products. Modern medical research shows that fritillaria ussuriensis mainly contains alkaloid components and has more remarkable pharmacological effects of relieving cough, eliminating phlegm, relieving asthma, resisting ulcer, resisting platelet aggregation, resisting inflammation and the like.
The Shennong Bencao Jing (Shennong's herbal) lists the fritillary as a middle-quality product, records that the fritillary has pungent and even flavor and no toxicity, and has main typhoid, dysphoria, stranguria with pathogenic factors, hernia symptoms, pharyngitis and milk difficulty, later generations of herbal are recorded in Tang Dynasty ' Xinhuibao ', Song Dynasty's herbal [ herbal Bo of Tu Jing Ben (St. herbal) and Ming Dynasty's era ' Ben Biao ', but all are called fritillary, and are not classified, until four years in Ming Tian Qi (1596 years) Zhen Cao (herbal Hui Yan), the best record of Sichuan person is provided for the fritillary prescription, and the best record of Sichuan person is provided for the Zhe fritillary in Qing Qianlong (1755) in Zhao Zhen Cao Zhen mu, and traditional fritillary bulb, and has the effects of moistening lung, heart meridian, phlegm reduction, dispersing and cough relieving. Pingbu Bei mu is classified as Taiyin ren Yao in the classic oriented medicine of Dong Yi shou Shi Bao Yuan (east medical science and Life preservation). Modern medical research shows that fritillaria ussuriensis contains alkaloids, alkaloid glycosides and nucleoside components, has obvious pharmacological effects of relieving cough, eliminating phlegm, relieving asthma, resisting ulcer and the like, and is listed in the catalog of health food raw materials. The fritillary bulb has higher asexual propagation coefficient than other fritillary bulbs, occupies an important position in the cultivation of fritillary bulbs in China, is commonly used for replacing the fritillary bulbs and the thunberg fritillary bulbs in northeast, and relieves the market supply. At present, the production technology and cultivation technology of fritillaria ussuriensis are increasingly mature, a large number of fritillaria ussuriensis are planted in mountainous areas of the northeast three provinces, and the yield is improved year by year.
The immunity is a defense mechanism of a human body, and the human body recognizes and eliminates any foreign matters (viruses, bacteria and the like) invaded from the outside; the ability to treat senescent, damaged, dead, degenerating self-cells, and to recognize and treat mutant and virally infected cells in vivo. Modern immunology considers that immunity is the physiological response of the human body to recognize and eliminate "isohexia".
According to traditional Chinese medicine, the term "immunity" is originally found in the "immunity prescription" of the Ming dynasty medical book of China, and means "avoiding pestilence", that is, the meaning of preventing and treating infectious diseases. The traditional Chinese medicine considers that the immunity is low, namely the healthy qi is lost, and the internal classic points out that: the healthy qi is retained in the interior and the pathogenic factors are not dried, but the qi is weakened. Strengthening healthy qi to eliminate pathogens and regulating yin and yang to improve immunity is the basis of strengthening immunity, and strengthening healthy qi refers to strengthening healthy qi of antibodies, and the deficiency of regulating and raising the meridians of internal organs, qi, blood and body fluids of human bodies through tonifying and strengthening directions so as to improve the disease resistance of the antibodies, improve the immune function of the antibodies and enhance the stability of the antibodies, so-called 'vigorous pathogen self-elimination'; the elimination of pathogenic factors is a traditional Chinese medicine treatment principle of eliminating pathogenic qi and eliminating or weakening invasion and damage of pathogenic factors, namely that' eliminating pathogenic factors leads to healthy qi and calm. Strengthening body resistance and eliminating pathogenic factors complement each other, and can enhance immunity of human body.
The Korean medicine and pharmacology gradually forms and develops by absorbing the theory of traditional Chinese medicine and pharmacology and combining the experience of preventing and treating diseases of the national nationality on the basis of the inherent culture and east medicine of the Korean nationality. The dynasties of medicine and pharmacology is the diagnosis and treatment theory which is guided by the overall view of "heaven, man, world and earth" and mainly takes the structure of "four-dimensional four-image" as the main form and combines the differentiation of image (constitution and disease) with the differentiation of symptoms and signs. The theory of "four elephants medicine" in medicine and pharmacology holds that "taiyin" is over 50% in four elephants, all the symptoms of taiyin are determined by the constitutional preponderance of taiyin, and the fundamental treatment of taiyin is to dispel the cold excessiveness to ensure that taiyin is healthy and disease-free. Towards medical science, all diseases are considered to be "nourished" rather than "treated". Therefore, in order to enhance immunity, it is necessary to nourish the five internal organs, regulate qi, eliminate stagnation, regulate yin and yang, tonify kidney, replenish qi, consolidate constitution and cultivate primordial qi.
The formula of the health food of the invention takes ginseng and fritillaria ussuriensis as raw materials, and auxiliary materials or auxiliary components acceptable for the health food are added. In the formula, ginseng is a new resource food, fritillaria ussuriensis is an article which can be used as a health food, and the composition of all raw materials meets the requirements of the health food on the source of the raw materials.
Among the raw materials, the ginseng has the effects of greatly reinforcing primordial qi, recovering pulse, relieving depletion, tonifying spleen, benefiting lung, promoting the production of body fluid, nourishing blood, calming nerves and benefiting intelligence; the fritillary bulb has the effects of clearing heat, moistening lung, reducing phlegm, relieving cough and the like. The fritillary bulb is matched with the ginseng, has the functions of clearing lung, moistening lung and tonifying lung qi, is clinically used for respiratory system diseases and various symptoms caused by weak lung function and reduced immunity, and has definite curative effect. The formula of the invention provides a new choice for developing health-care food.
The function evaluation experiment proves that the health food has the function of enhancing immunity, can obviously regulate the humoral immunity and the cellular immunity of the organism, and enhances the activity of natural killer cells.
At present, no health food based on the Chinese medical health-preserving theory is listed on the market, no health food patent and research report similar to the formula of the composition are found by searching Chinese patent and literature database, and the design theory and thought of the composition are innovative. The health food with the function of enhancing immunity is developed on the basis of the invention, and has wide market demand prospect.
Disclosure of Invention
The technical scheme of the invention provides a health food composition which takes ginseng and fritillaria ussuriensis as main raw materials of a formula under the guidance of the medicine theory, and the health food composition has the function of enhancing immunity. The invention also provides a preparation method of the health food.
The invention provides a health food composition with the function of enhancing immunity, which is prepared from the following raw materials in parts by weight: 1-4 parts of ginseng and 1-3 parts of fritillary bulb.
Further preferably, the feed additive is prepared from the following raw materials in parts by weight: 4 parts of ginseng and 3 parts of fritillary bulb.
The health food is a preparation prepared by taking fritillaria ussuriensis extract and fine ginseng powder as active ingredients and adding auxiliary materials or auxiliary ingredients acceptable for health food.
Wherein, the preparation is as follows: granules, capsules and tablets.
The invention also provides a preparation method of the health food, which comprises the following steps:
(1) preparing raw materials: the fritillary bulb and the ginseng are weighed according to the formula of the health-care food composition, and the quality of the raw materials conforms to the regulation of 2015 edition (part one) of pharmacopoeia of the people's republic of China.
(2) Ginseng crushing: pulverizing Ginseng radix, sieving with 120 mesh sieve to obtain Ginseng radix fine powder and Ginseng radix coarse powder not passing through 120 mesh sieve.
(3) Extracting fritillary bulb: extracting with 40-90% ethanol for 2 times at a ratio of 1:10 and 1:8 for 2h and 1h, filtering, and mixing filtrates to obtain extractive solution I.
(4) Extracting ginseng: extracting the ginseng coarse powder for 2 times at room temperature by adopting an ultrasonic circulation method, wherein the interval ultrasonic ratio is 0.6s:0.5 s-0.6 s:4.5s, and the power is 300-700W; for the first time, water is used as a solvent, and the ratio of material to liquid is 1: 10-1: 12, and the extraction time is 0.5-1.5 h; and taking 60-85% ethanol as a solvent for the second time, wherein the ratio of material to liquid is 1:8, extracting for 0.5 h; centrifuging the extracted material liquid, filtering the supernatant to obtain filtrate, collecting the first filtrate to obtain extract II, and collecting the second filtrate to obtain extract III for use.
(5) Collecting paste: mixing the extract I and the extract II, concentrating under reduced pressure, drying at low temperature, and pulverizing to obtain extract powder; or spray drying to obtain extract powder.
(6) Preparing a soft material: and (3) taking the ginseng fine powder, adding the auxiliary materials and the extract powder in an equal amount, gradually mixing, adding the extracting solution III serving as a bonding agent, and kneading to obtain the soft material.
(7) Granulating and finishing: and (3) taking the soft material, putting the soft material into a granulator for granulation to obtain wet granules, taking the wet granules for boiling drying, and finishing granules after drying to obtain dry granules.
(8) Molding: filling the dry granules into an aluminum-plastic packaging bag to obtain granules; filling into empty capsule to obtain capsule; adding filler, disintegrant or correctant, granulating, and tabletting to obtain tablet.
(9) Packaging and labeling to obtain the final product.
The composition of the invention is mainly used for health-care food which is helpful for enhancing the immunity function.
The preparation method of the invention is mainly used for producing the solid preparation taking ginseng and fritillaria ussuriensis as raw materials.
Detailed Description
The present invention will be described in more detail with reference to the following examples and examples.
Experimental example 1 study on method for measuring content of total alkaloids in fritillary bulb
The total alkaloid content is taken as an evaluation index. And (3) establishing an acid dye colorimetric method to determine the content of the total alkaloids in the fritillaria ussuriensis.
Preparation of the solution
Buffer solution: taking 0.2 mol.L-1Potassium hydrogen phthalate solution 100mL(4.08 g) with 0.2 mol. L-1Adjusting pH to 5.0 with about 50mL (0.4 g) of sodium hydroxide solution to obtain the final product.
Bromthyme finnish solution: 0.03g of bromothymol blue is weighed and dissolved in 0.5mL of 1 mol.L-1Adding distilled water into the sodium hydroxide solution to dilute the solution to 100mL, and shaking the solution uniformly to obtain the sodium hydroxide.
Control solution: 2.55mg of peimine as a reference substance was weighed precisely and dissolved in a 25mL volumetric flask with chloroform as a reference solution.
Preparation of sample solution: 2.00g of fritillary bulb powder (sieved by a 65-mesh sieve) is precisely weighed and prepared according to the related requirements of pharmacopeia.
Determination of detection wavelength
Precisely sucking 4.0mL to 25mL of the peimine reference substance solution in a volumetric flask, adding 5mL of buffer solution with pH =5 and 2mL of bromothymol blue test solution, adding chloroform to a constant volume, fully shaking up, transferring into a separating funnel, and standing for 45 min. Filtering the chloroform layer (subnatant) with dry filter paper, collecting the subsequent filtrate, adjusting the blank with chloroform, and measuring the absorbance at 350-500 nm of an ultraviolet-visible spectrophotometer.
The measurement result shows that the control solution has maximum absorption at 408-412nm, and 410nm is selected as the measurement wavelength.
Investigation of Linear relationships
Precisely sucking peimine reference substance solution 1.0, 2.0, 3.0, 4.0, 5.0 mL-25 mL respectively, performing colorimetric determination of alkaloid content and absorbance relationship according to 2.2 method, and determining peimine content (mg. mL. mL)-1) The abscissa and the ordinate represent absorbance, and a standard curve is prepared. The regression equation is obtained as: y =0.0424X +0.1454, r = 0.9908. The result shows that the concentration of the peimine is 0.004-0.020 mg/mL-1The linear relationship within the range is good.
Precision survey
Accurately sucking 5mL of the peimine reference substance solution, carrying out colorimetric determination according to the method under item 2, repeatedly determining for 5 times, and calculating the RSD value to be 0.086% (n = 5) according to the absorbance value, thereby indicating that the precision of the instrument is good.
Stability survey
The sample solution was precisely aspirated by 5mL, and colorimetrically measured at 0, 2, 4, 6, and 8h at room temperature by the method under item 2, and RSD value calculated as absorbance value was 2.04% (n = 5), indicating that the sample solution was stable within 8 h.
Repeatability survey
The sample solution (5 mL) was precisely aspirated, the colorimetric measurement was performed by the method described in item 2, the measurement was repeated 5 times, and the RSD value was 1.53% (n = 5) as the absorbance value, indicating that the method was excellent in precision.
Determination of medicinal material content
Respectively and precisely weighing 5 parts of fritillary bulb medicinal material, measuring according to the method under 2 items, calculating the total alkaloid content in the fritillary bulb medicinal material according to the following formula, namely the peimine is 0.237%, and the RSD value is 1.43% (n = 5), and the results are shown in table 1.
TABLE 1 measurement results of the contents of the herbs
Figure 46268DEST_PATH_IMAGE001
Figure 337572DEST_PATH_IMAGE002
(y-Absorbance, n-dilution factor, w-sample mass g)
Experimental example 2 research on extraction process of total alkaloids in fritillary bulb
An ethanol reflux extraction method is adopted, the total alkaloid extraction amount is taken as an evaluation index, and extraction process parameters such as material-liquid ratio, extraction time, ethanol concentration and the like are optimized through orthogonal experimental design.
Raw material treatment
Removing impurities from Bulbus Fritillariae Ussuriensis, cleaning, oven drying, and mashing to obtain coarse powder.
Extract sample preparation
Fritillary bulb coarse powder → ethanol reflux extraction for 2 times → filtration, merging the two filtrates → filtrate decompression concentration, evaporation to dryness → residue adding chloroform to fix the volume to a 25mL volumetric flask → precisely measuring the volume to a 2mL to 25mL volumetric flask.
Design of single factor test
3.1 selection of extraction solvent
2 parts of fritillary bulb coarse powder is precisely weighed, 10.00g of each part is respectively soaked in water and 70% ethanol for 1 hour, the fritillary bulb coarse powder is heated, decocted and extracted twice, the time is respectively 1.5 hour and 1 hour, the material-liquid ratio is respectively 1:10 and 1:8, the extraction is carried out according to the method under 2 items, the absorbance is measured according to the determination of the detection wavelength in the experimental example 1, and as a result, the effect of ethanol on extracting the total alkaloids is better, so that the ethanol extraction with a certain concentration is more suitable.
Examination of immersion time and Water absorption
Adding 70% ethanol in an amount which is 10 times that of fritillary bulb crude powder, soaking, draining off the solvent every 15min, and weighing the medicine residues until the weight of the medicine residues is unchanged. As a result, the medicinal materials can completely absorb water within 1h, and the weight of the medicinal materials does not change any more, so that the soaking time is set to 1h, and the water absorption rate of the medicinal materials is 173.37%.
Design of orthogonal experiments
Taking total alkaloid content (expressed by absorbance value) in extractive solution as index, and adopting L9(33) Orthogonal test table, based on single factor test result and relevant literature, 3 extraction process parameters of solvent dosage, extraction time and ethanol concentration are optimized, the factors and levels are shown in table 2, and the test arrangement and results are shown in table 3.
The method comprises the following steps: accurately weighing appropriate amount of Bulbus Fritillariae Ussuriensis coarse powder, preparing extractive solution sample according to the above method according to orthogonal test scheme, and measuring total alkaloid content (expressed by absorbance value) in the sample.
TABLE 2 orthogonal test design factor horizon
Figure 604605DEST_PATH_IMAGE003
TABLE 3 orthogonal test arrangement and results
Figure 272347DEST_PATH_IMAGE004
5 analysis of orthogonal test results
The extraction rate of total alkaloids (expressed by absorbance value) is taken as a survey index, the result of the anova is shown in Table 4, the result shows that the factor A, B has no significant influence on the extraction rate of the total alkaloids, and the factor C has significant influence on the extraction rate of the total alkaloids (p)<0.05), the main and secondary action of each factor is C>A>>And B, further determining the optimal extraction scheme, and performing multi-level mean value test. The results show that A3>A1>A2 ,B2>B1>B3 ,C3>C2>C1Therefore, the optimal extraction scheme from the above analysis is A3B2C3,Namely, the dosage of the solvent is 10, 8 times; the extraction time is 2, 1 h; the ethanol concentration was 80%.
TABLE 4 analysis of variance results
Figure 410067DEST_PATH_IMAGE005
6 validation test
Weighing appropriate amount of 3 parts of medicinal materials in the same batch, and performing optimal process A3B2C3The tests were carried out and the results are shown in Table 5.
Table 5 verifies the test results
Figure 403431DEST_PATH_IMAGE006
As a result, the extraction rates of the total alkaloids are 86.08%, 84.81% and 83.12%, the average extraction rate is 84.67% and the RSD value is 0.02%, which shows that the optimized extraction process is stable and feasible.
The fritillary bulb extracting solution prepared by the method is the extracting solution I.
Experimental example 3 study of Ginseng radix processing technology
The monarch drug in the composition is ginseng, and the ginseng is a valuable medicinal material, so the formula adopts the mode that the ginseng is crushed and sieved, fine powder is directly used as the medicine, and coarse powder is further extracted to comprehensively utilize the ginseng. The method comprises the following steps: pulverizing Ginseng radix, sieving with 120 mesh sieve, collecting fine powder, and extracting coarse powder.
3.1 investigation of the powder yield of ground Ginseng
The ginseng was pulverized by a universal pulverizer, and the powder was sieved through a 120-mesh sieve to examine the powder yield, and the results are shown in table 6. The result shows that the powder yield of the ginseng fine powder crushed according to the method is 87.04%.
TABLE 6 examination of the powder yield
Figure 875870DEST_PATH_IMAGE007
3.2 study of extraction Process of Ginseng radix coarse powder
Pharmacological research shows that the total ginsenoside is one of the effective components of ginseng in raising body's immunity. Therefore, the extraction of the ginseng in the experiment takes the total saponins of the ginseng as an index, and the extraction process of the ginseng is researched.
3.2.1 methodology investigation
Measuring total saponin by ultraviolet spectrophotometry.
3.2.1.1 preparation of the solution
(1) Precisely weighing 1.0 g of ginseng in a sample solution, placing the ginseng in a 100mL volumetric flask, adding a small amount of water, carrying out ultrasonic treatment for 30min, then adding water to a constant volume of 100mL, shaking up, placing, and absorbing 1mL of supernatant for column chromatography.
(2) Column chromatography: a column with an inner diameter of 2 cm is used as a chromatography tube, 3 cm Amberlite-XAD-2 macroporous resin is filled in the chromatography tube, and 1 cm neutral alumina is added on the macroporous resin. Eluting the column with 25mL of 70% ethanol, discarding the eluate, eluting the column with 25mL of water, discarding the eluate, precisely adding 1mL of the treated sample solution (see 1.1), eluting the column with 25mL of water, discarding the eluate, eluting ginsenoside with 25mL of 70% ethanol, collecting the eluate, evaporating in an evaporation dish, and evaporating in a water bath at 60 deg.C. Thereby, the color is developed.
(3) Color development: accurately adding 5% vanillin glacial acetic acid solution into the evaporated evaporation pan, rotating the evaporation pan to dissolve the residue, adding 0.8 mL perchloric acid, mixing, transferring into 5mL centrifuge tube with plug, heating in water bath at 60 deg.C for 10 min, taking out, cooling in ice bath, accurately adding glacial acetic acid 5.0mL, shaking, and performing colorimetric determination with standard tube at 560 nm wavelength in 1 cm cuvette.
(4) Standard tubes: 100 ul of ginsenoside Re standard solution (2.0 mg/mL) was taken and placed in an evaporation dish, and the evaporation dish was placed in a water bath to evaporate (below 60 ℃) or dried with hot air (without overheating), and the procedure was the same as that of the sample from the point of column chromatography. The absorbance values were determined.
3.2.1.2 Linear relationship examination 0.12, 0.14, 0.16, 0.18, 0.20, 0.22 mg of the control solutions were taken in 10mL volumetric flasks, methanol was added to the scale, shaking was carried out, and the absorbance at 560 nm was measured. Linear regression was performed with the control solution concentration (X) and absorbance value (Y) to give the regression equation Y = 4.9943X-0.1737, r =0.9997 (n = 6). The results show that the control concentration and absorbance values are in good linear relationship in the range of 0.012-0.022 mg/mL.
3.2.1.3 precision investigation precision absorption of the control solution, repeated 5 times, the result RSD value of 0.14%, indicating good precision of the instrument.
3.2.1.4 stability examination the test solution was precisely aspirated for 0, 2, 4, 6, 8, 10, 12h, and the absorbance was measured, with the result that the RSD value was 1.81%, indicating that the test solution was stable within 12 h.
3.2.1.5 repeatability examination precisely measures the same batch of sample, prepares 5 test samples according to the test solution item, and measures the absorbance. The result RSD value is 0.45%, which shows that the method has good repeatability.
3.2.1.6 sample application recovery rate examination 6 portions of sample solution with known content were precisely measured, and appropriate amount of reference substance was precisely added, respectively, and prepared under the test solution, and the recovery rate was calculated, and the results are shown in Table 7. The result shows that the average recovery rate of the method is 100.21%, and RSD = 1.41%, which indicates that the method has better accuracy and is feasible.
TABLE 7 results of sample recovery test
Figure 347302DEST_PATH_IMAGE008
3.2.1.7 sample assay
The content of 3 batches of medicinal material samples is measured according to the measuring method, and the result is shown in table 8.
TABLE 8 determination of total saponin content in three batches of medicinal material samples
Figure 870687DEST_PATH_IMAGE009
3.2.2 optimization of extraction Process
3.2.2.1 influence of extraction solvent on total saponin extraction rate 4 groups of ginseng coarse powder are taken, different solvents are added, ultrasonic extraction is carried out for 1h under the conditions of ultrasonic power of 500W and interval ultrasonic time ratio of 0.6:1.5 s and room temperature, filtration is carried out to obtain extracting solution, and the content of total saponin is determined according to the method. The results show that the extraction solvent is best extracted with water, see table 9.
TABLE 9 Total Saponin extraction yield results from three different solvents
Figure 503794DEST_PATH_IMAGE010
3.2.2.2 influence of feed liquid ratio on total saponin extraction rate 3 groups of ginseng coarse powder are taken, each group comprises 3 parts of each group, each group comprises 150 g, water is taken as an extraction solvent, the raw materials and the extraction solvent are respectively mixed according to the ratio of 1:10, 1:12 and 1: 14, the extraction is carried out under the condition of 3.2.1, the content of the total saponin is determined, and the result shows that the feed liquid ratio has influence on the total saponin extraction rate, the extraction rate is 1:12, the extraction rate is approximate to 1: 14 and is obviously higher than 1:10, so the feed liquid ratio is determined to be 1: 12.
3.2.2.3 influence of ultrasonic technological parameters on Total Saponin extraction yield by selecting interval ultrasonic time ratio (A) Extraction time (c)B) Ultrasonic power (C)C) For inspecting factors, the extraction rate is used as an evaluation index, and an orthogonal design test is adopted to optimize process parameters. The factor levels are shown in Table 10, the test schedule is shown in Table 11, and the results of the ANOVA are shown in Table 12. Taking ginseng coarse powder, adding 12 times of water, extracting according to the scheme in the table 11, filtering an extracting solution, fixing the volume of a filtrate to be a sample solution, and measuring the content of total saponins. The total saponin extraction rate was calculated and the results are shown in table 11. The results show that within the selected level rangeA、B、C The influence degree of the 3 factors on the extraction rate is consistent, and no significant difference exists. According to the visual experiment result, the optimal technological parameters are determined to beA 1 B 2 C 2 Namely, the ultrasonic time interval ratio is 0.6: 0.5, the extraction time is 1h, and the ultrasonic power is 500W.
TABLE 10 orthogonal design test factors and levels
Figure 214261DEST_PATH_IMAGE011
TABLE 11 orthogonal design test arrangement and results
Figure 754964DEST_PATH_IMAGE012
TABLE 12 results of ANOVA
Figure 349500DEST_PATH_IMAGE013
3.2.3 validation experiment Ginseng radix coarse powder was extracted according to the preferred process conditions and subjected to 3 parallel experiments. As a result, the total saponin extraction rate is 88.58% which is close to the maximum value of the orthogonal design test, and the optimal process parameters are reasonable.
3.2.4 the above experiments have certain limitations by using the content of ginsenoside as the index component of the ginseng extraction process, and the ginseng contains various other active components besides the saponin, so that other effective components (such as fat-soluble components) in the ginseng can be fully extracted, and the extraction process is finally determined as follows: extracting twice at room temperature by an ultrasonic circulation method, wherein water is used as a solvent for the first time, the material-liquid ratio is 1:12, and the extraction time is 1h, so that an obtained extracting solution is an extracting solution II; taking 70% ethanol as a solvent for the second time, wherein the ratio of material to liquid is 1:8, extracting for 0.5h to obtain an extracting solution III; ultrasonic technological parameters are as follows: the interval ultrasonic ratio is 0.6s to 0.5s, and the power is 500W.
Experimental example 4 research on forming process of preparing dispersible tablet from health food of the present invention
The novel solid preparation has simple production process, has no special requirement on production conditions, is substantially the same as the common tablet production process, has the characteristics of low production cost, high disintegration speed, high bioavailability, convenient taking and the like, and is particularly suitable for old, young and people who have difficulty in swallowing the medicine. The preparation of the dispersible tablet focuses on the screening of preparation auxiliary materials.
4.1 preparation method
4.1.1 preparation of extract powder
Mixing extractive solution I and II, concentrating under reduced pressure, drying at low temperature, pulverizing to obtain extract powder, or spray drying to obtain extract powder with calculated extract yield of 15%
4.1.3 granulating and tabletting
Mixing Ginseng radix fine powder, extract powder and adjuvants, adding extractive solution III as binder, kneading to obtain soft material, granulating in granulator, drying wet granules, sieving with 16 mesh sieve, and grading to obtain dry granules; tabletting with tabletting machine (¢ 20 mm circular punch) to obtain dispersible tablet.
4.2 adjuvant screening
The prescription screening of the preparation is carried out by taking the appearance, hardness and disintegration time of the dispersible tablet as indexes, and the comprehensive scoring standard is shown in table 13.
TABLE 13 general Scoring Standard for dispersible tablets of Ginseng and Bei
Figure 419087DEST_PATH_IMAGE014
4.2.1 Filler MCC, lactose, starch 3 commonly used fillers were screened. The adjuvants are sieved with 100 mesh sieve, and granulated and tabletted with L-HPC (raw material: L-HPC =1: 0.2) as disintegrant and 70% ethanol solution as binder, and the appearance is observed, and the hardness and disintegration time are measured, the result is shown in Table 14, so MCC is selected as dispersible tablet filler finally.
TABLE 14 tabletting test results for different fillers
Figure 882429DEST_PATH_IMAGE015
4.2.2 disintegrating agent L-HPC, PVPP two kinds of disintegrating agent were screened, the supplementary material was sieved with 100 mesh sieve, MCC was used as filler, the two kinds of disintegrating agents were used in the same amount, 70% ethanol solution was used as binder, the appearance was observed, and the hardness and disintegration time were measured, and the results are shown in Table 15. Therefore, PVPP is finally selected as the disintegrating agent of the dispersible tablet.
TABLE 15 results of different disintegrant tableting experiments
Figure 695665DEST_PATH_IMAGE016
4.2.3 wetting agent the material before forming of the preparation of the invention contains a large amount of sugar, so that the extract powder has a large viscosity, and the extract powder has too strong viscosity when meeting water and is not easy to granulate, so 40%, 50%, 60% and 70% ethanol solutions are respectively adopted as the wetting agent. As the concentration of ethanol increases, the viscosity produced upon wetting decreases. 40 percent, 50 percent and 60 percent of ethanol are used as wetting agents, the powder has larger viscosity, the powder is easy to agglomerate, 70 percent of ethanol is used as the wetting agent, the powder has moderate viscosity, and the powder is easy to be made into soft materials. Therefore, the extracting solution III in the research of the extracting process of the invention is an adhesive (the concentration of ethanol is about 70 percent), the viscosity of the extract can be properly reduced, the powder is not too loose, and the soft material is easy to prepare; meanwhile, the extracting solution is used as an adhesive, so that the using amount of auxiliary material ethanol can be saved.
4.3 tabletting and forming process
4.3.1 determination of various indexes of the dry granules
4.3.1.1 measurement of fluidity, particle size distribution and water content according to the requirements of Chinese pharmacopoeia (2015 edition) (four parts). The angle of repose was determined by the fixed funnel method for fluidity, the distribution ratio was determined by the sieving method for particle size distribution, the moisture content was determined by the drying method, and the results are shown in Table 16.
Table 16 dry granules each index measurement result (n = 3)
Figure 928063DEST_PATH_IMAGE017
4.3.1.2 hygroscopicity was measured according to the requirements of the Chinese pharmacopoeia (15 th edition) (four parts). And calculating the moisture absorption weight gain percentage and drawing a moisture absorption curve. The results show that the particles are balanced by moisture absorption after being left for 5 days under the condition that the relative humidity is 42 percent.
4.3.2 calculate the tablet weight before tabletting, which can be calculated according to the following formula.
Theoretical tablet weight = (main drug amount/main drug proportion in tablet)/number of tablets taken per day
=(1.65 / 0.56)/ 6 = 0.49g
The actual dosage is about 0.5g per tablet, and 6 tablets are taken in a day, and the dosage is divided into 3 times, which accords with the health food regulation.
4.4 conclusion
The formula of the dispersible tablet preparation comprises raw materials, MCC and PVPP (5: 3: 1), and III containing 70% ethanol is a wetting agent. The auxiliary materials and the proportion screened by the method are produced in batches, the appearance, the properties, the weight difference, the hardness and the content of the auxiliary materials all meet the requirements, and the process conditions are proved to be stable, reasonable and feasible.
Experimental example 5 research on quality standards of dispersible tablets prepared from the health food of the present invention
5.1 authentication
5.1.1 thin layer identification of Ginseng radix, and adding methanol to obtain 2mg/ml solution of ginsenoside Rb1, ginsenoside Rg1, ginsenoside Rf, and ginsenoside Re. Taking 1g of the product powder, adding 40ml of trichloromethane, heating and refluxing for 1h, discarding trichloromethane liquid, volatilizing the solvent in the medicine residue, adding 0.5ml of water, stirring and wetting, adding 10ml of water saturated n-butyl alcohol, carrying out ultrasonic treatment for 30min, sucking the supernatant, adding three times of ammonia solution, shaking uniformly, standing for layering, taking out the supernatant, evaporating to dryness, and dissolving the residue in 1ml of methanol to obtain the sample solution. Chloroform-ethyl acetate-methanol-water (15: 40: 22: 10), left at 10 ℃ or below for 12h, and the lower layer solution was taken as a developing agent. Developing with chloroform-ethyl acetate-methanol-water (15: 40: 22: 10) as developing agent, taking out, air drying, spraying 10% ethanol sulfate solution, heating at 105 deg.C until the spots are clearly developed, and observing under 365nm ultraviolet lamp. In the chromatogram of the test solution, spots with the same color appear at the positions corresponding to those in the chromatogram of the control solution, and no spot appears in the negative control solution.
5.1.2 identification of Bulbus Fritillariae Ussuriensis, the product powder 10g is added with concentrated ammonia solution 10ml and chloroform solution 30ml, ultrasonic treatment is carried out for 30min, filtration is carried out, filtrate is evaporated to dryness, and methanol solution 0.5ml is added into residue to dissolve it to obtain test solution. Taking 10g of Bulbus Fritillariae Ussuriensis as reference medicinal material, and making into reference medicinal solution by the same method. Developing with ethyl acetate-methanol-concentrated ammonia-water (10: 1:0.5: 0.5) as developing agent, taking out, air drying, spraying with bismuth potassium iodide solution and sodium nitrite ethanol solution, and heating at 105 deg.C until the spots are clearly developed. In the chromatogram of the test solution, fluorescent spots with the same color appear at the corresponding positions of the chromatogram of the control solution, and the negative control solution has no corresponding spots.
5.2 determination of Total Alkaloids in dispersible tablets
Measuring total alkaloid content in dispersible tablet by ultraviolet spectrophotometry.
5.2.1 preparation of the solution
(1) Precisely weighing 2.5mg of peimine reference substance, adding chloroform to a volumetric flask with a constant volume of 25ml, and shaking up to obtain 0.1mg/ml reference substance stock solution.
(2) Taking the powder of the test solution, precisely weighing, placing in a conical bottle with a plug, adding 3ml of concentrated ammonia, soaking for 1h, adding trichloromethane: 40ml of methanol (4: 1) mixed solution is put into a water bath kettle at 80 ℃ for refluxing for 2 h. Cooling, filtering, washing the dregs of a decoction for 2-3 times by using the mixed solution, and combining the filtrates. Evaporating to dryness, and adding chloroform solution into the residue to constant volume of 25ml to obtain the final product.
(3) Taking 100ml of potassium hydrogen phthalate solution, and adjusting the pH value to 5.0 by using about 50ml of 0.2mol/L sodium hydroxide solution to obtain the potassium hydrogen phthalate solution.
(4) Bromthymph Finnish solution 0.03g of bromothymus Finnish was weighed out accurately, dissolved in 0.5ml of 1mol/L sodium hydroxide solution and diluted to 100ml with water.
5.2.2 Linear relationship examination precisely measured 0ml,0.5ml,1ml,2ml,3ml and 4ml of the peimine reference substance solution in a 25ml volumetric flask, respectively adding 5ml of 0.2mol/L potassium hydrogen phthalate buffer solution and 2ml of bromothyme fenland solution, adding trichloromethane solution to a constant volume to a scale, violently shaking, transferring to a separating funnel, standing for 45min, filtering with dry filter paper, and taking the subsequent filtrate of the trichloromethane layer. The absorbance was measured under UV light at a wavelength of 412 nm. Performing linear regression with the concentration (X) of the control solution as abscissa and the absorbance value (Y) as ordinate to obtain regression equation of Y = 2.0494X + 0.0586,r = 0.9996(n = 6), indicating that the control concentration has a good linear relationship with the absorbance value in the range of 0.002-0.016 mg/L.
5.2.3 precision survey the precision measured reference solution, repeat the measurement 5 times, the result RSD value is 0.14%, indicating that the precision of the instrument is good.
5.2.4 stability evaluation test solutions were precisely measured and absorbance was measured at 0, 2, 4, 6, 8, 10, and 12 hours, respectively, and the RSD value was 1.161%. The test solution is stable within 12 h.
5.2.5 repeatability examination precisely weighing the same batch of samples, preparing 5 parts of test sample according to the test sample solution item, and measuring the absorbance. The RSD value was 1.883%. The method has good repeatability.
5.2.6 sample application recovery Rate 6 portions of sample solution with known content were measured precisely, and appropriate amount of control was added precisely, respectively, and prepared under the test solution, and the recovery rate was calculated, the results are shown in Table 17. The result shows that the average recovery rate of the method is 99.92, and RSD = 0.6581%, which indicates that the method has better accuracy and is feasible.
TABLE 17 examination of sample recovery
Figure 168551DEST_PATH_IMAGE018
5.2.7 content measurement of samples 3 batches were measured according to the above measurement method and the content was calculated, and the results are shown in Table 18. According to the content measurement results of 3 batches of samples, the content of total alkaloid in each 1g of provisional product is not less than 1.35 mg (according to 1.495mg multiplied by 90%).
TABLE 18 measurement results of sample content
Figure 837299DEST_PATH_IMAGE019
5.3 ginsenoside Rg in dispersible tablet1Ginsenoside Re and ginsenoside Rb1Determination of content
Determining ginsenoside Rg in dispersible tablet by high performance liquid chromatography1Ginsenoside Re and ginsenoside Rb1The content of (a).
5.3.1 chromatographic condition the chromatographic column is Thermo ODS-2HYPERSIL (4.6 mm. times.250 mm, 5 um), the mobile phase is mobile phase acetonitrile-water, the flow rate is 1 ml/min; the detection wavelength is 203nm, and the column temperature is 30 ℃. Gradient elution was performed according to the mobile phase conditions of Table 19. The number of theoretical plates is not less than 6000 according to the peak of ginsenoside Rg 1.
TABLE 19 conditions of mobile phase
Figure 188646DEST_PATH_IMAGE020
5.3.2 preparation of solutions
Mixing the reference solution: precise weighing of ginsenoside Rg1Reference substance, ginsenoside Rb1Adding appropriate amount of reference substance and ginsenoside Re reference substance into methanol to obtain mixed solution with concentration of 0.1mg/ml, 0.2mg/ml, 0.3mg/ml, 0.4mg/ml, and 0.5 mg/ml.
Test solution: precisely weighing about lg (passing through a sieve of No. four), placing in a Soxhlet extractor, adding a trichloromethane solution, refluxing for 3 hours under a heating state, discarding the trichloromethane solution, volatilizing the solvent of the decoction dregs, transferring into a 100ml conical flask together with a filter paper cylinder, precisely adding 50ml of a water saturated n-butyl alcohol solution, sealing, standing overnight, carrying out ultrasonic treatment for 30 minutes under the conditions of the power of 250W and the frequency of 50kHz, filtering, discarding an initial filtrate, precisely measuring 25ml of a subsequent filtrate, placing in an evaporating dish, evaporating to dryness, dissolving the residue with methanol, transferring into a 5ml measuring flask, adding methanol to dilute to a scale, shaking uniformly, filtering, and taking the subsequent filtrate.
5.3.3 systematic applicability test reference substance solution is injected into 10ul, and measured, the retention time of ginsenoside Rg1 reference substance, ginsenoside Rb1 reference substance and ginsenoside Re under the condition of the chromatogram is 14.2, 14.9 and 64.9min respectively, and the theoretical plate number is Rg1The peak was calculated to be not less than 6000.
5.3.4 Linear relationship investigation of each concentration of control solution, respectively injecting 10ul of sample, determining peak area, and performing regression on the sample injection amount (X) with the peak area (Y), wherein ginsenoside Rg1: y =66158X-15463, r =0.9998 (n = 6), ginsenoside Re: y =73265X-4443, r =0.9997 (n = 6), ginsenoside Rb1: the results of Y =58930X-11579 and r =0.9997 (n = 6) show that the sampling amount of 3 ginsenosides is in good linear relation with the peak area in the range of 1.0-5.0 ug.
5.3.5, respectively inspecting the precision, stability and repeatability, and the result shows that the precision of the instrument is good, and the solution of the test sample is stable within 12h and has good repeatability.
5.3.8 investigation of sample recovery rate1Ginsenoside Re and ginsenoside Rb11g of the health food with the contents of 1.321 mg/g, 2.241 mg/g and 1.658 mg/g respectively for ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The RSD values are all less than 2 percent by carrying out sample-adding recovery rate inspection
5.3.9 the content determination of dispersible tablet sample precisely absorbs 10ul of each of the control solution and 3 batches of test solutions, and calculates the content of ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 by peak area through external standard method, and the result is shown in Table 20. The results show that the ginsenoside Rg in the dispersible tablets1Ginsenoside Re and ginsenoside Rb1The contents were 1.321 mg/g, 2.241 mg/g, and 1.658 mg/g, respectively.
TABLE 203 measurement of ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1 in the samples
Figure 541130DEST_PATH_IMAGE021
According to the content determination results of the 3 batches of samples, 1g of the product is tentatively determined to contain ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1Respectively not less than 1.89mg, 0.80mg, 1.47mg (90% by weight of each component), and each tablet is 0.5g, so that each tablet of the product contains ginsenoside Rg1, ginsenoside Re, and ginsenoside Rb1 respectively not less than 0.94mg, 0.40mg, and 0.74 mg.
Example 1 preparation of a health food composition of the present invention into granules
The formula is as follows:
the preparation method comprises the following steps:
(1) weighing the raw materials according to the weight ratio of the health food, taking ginseng, crushing and sieving, wherein ginseng fine powder passes through a 120-mesh sieve, and ginseng coarse powder which does not pass through the 120-mesh sieve are reserved;
(2) extracting fritillary bulb: extracting with 80% ethanol for 2 times at a ratio of 1:10 and 1:8 for 2h and 1h, filtering, and mixing filtrates to obtain extractive solution I. (ii) a
(3) Taking ginseng coarse powder, extracting twice at room temperature by adopting an ultrasonic circulation method, wherein water is used as a solvent for the first time, and the ratio of material to liquid is 1:10, the extraction time is 0.5h, 70% ethanol is used as a solvent for the second time, and the ratio of material to liquid is 1:8, extracting for 0.5h, wherein the ultrasonic interval ratio is 0.6s to 0.5s, the power is 500W, centrifuging the extracted feed liquid, filtering the supernatant to obtain a filtrate, collecting the first filtrate to obtain an extracting solution II, and collecting the second filtrate to obtain an extracting solution III for later use;
(4) mixing the extract I and the extract II, concentrating under reduced pressure, drying at low temperature, and pulverizing to obtain extract powder; or spray drying to obtain extract powder.
(5) Preparing a soft material: and (3) taking the ginseng fine powder, adding the auxiliary materials and the extract powder in an equal amount, gradually mixing, adding the extracting solution III serving as a bonding agent, and kneading to obtain the soft material.
(6) And (3) granulating: and (3) taking the soft material, putting the soft material into a granulator for granulation to obtain wet granules, taking the wet granules for boiling drying, and finishing granules after drying to obtain dry granules.
(7) And filling the dry granules into an aluminum-plastic packaging bag to obtain the granules.
EXAMPLE 2 preparation of dispersible tablets from the health food composition of the invention
The formula is as follows:
Figure 952520DEST_PATH_IMAGE022
the preparation method comprises the following steps:
(1) weighing the raw materials according to the weight ratio of the health food, taking ginseng, crushing and sieving, wherein ginseng fine powder passes through a 120-mesh sieve, and ginseng coarse powder which does not pass through the 120-mesh sieve are reserved;
(2) extracting fritillary bulb: extracting with 80% ethanol for 2 times at a ratio of 1:10 and 1:8 for 2h and 1h, filtering, and mixing filtrates to obtain extractive solution I. (ii) a
(3) Taking ginseng coarse powder, extracting twice at room temperature by adopting an ultrasonic circulation method, wherein water is used as a solvent for the first time, and the ratio of material to liquid is 1:10, the extraction time is 0.5h, 70% ethanol is used as a solvent for the second time, and the ratio of material to liquid is 1:8, extracting for 0.5h, wherein the ultrasonic interval ratio is 0.6s to 0.5s, the power is 500W, centrifuging the extracted feed liquid, filtering the supernatant to obtain a filtrate, collecting the first filtrate to obtain an extracting solution II, and collecting the second filtrate to obtain an extracting solution III for later use;
(4) mixing the extract I and the extract II, concentrating under reduced pressure, drying at low temperature, and pulverizing to obtain extract powder; or spray drying to obtain extract powder.
(5) Preparing a soft material: and (3) taking the ginseng fine powder, adding the auxiliary materials and the extract powder in an equal amount, gradually mixing, adding the extracting solution III serving as a bonding agent, and kneading to obtain the soft material.
(6) And (3) granulating: and (3) taking the soft material, putting the soft material into a granulator for granulation to obtain wet granules, taking the wet granules for boiling drying, and finishing granules after drying to obtain dry granules.
(7) And (4) putting the dry granules into a tabletting machine for tabletting to obtain the dispersible tablets.
Example 3 evaluation of the function of dispersible tablets prepared from the health food of the present invention
1 evaluation experiment of Immunity-enhancing function
1.1 test samples are three batches of dispersible tablets (20160403, 20160404, 20160405) produced according to the invention, each tablet of the product is 0.5g, the orally recommended dose is 6 tablets per day, the reduced dose is 0.05g/(kg.d) calculated according to the adult body weight of 60 kg, and 5, 10, 30 times of the administered dose is taken as the test object in the experiment.
The experimental animal is a male Kunming mouse.
Dose grouping and test sample administration time experiments 3 test subject groups, 1 negative control group were set up. The male Kunming mice were randomly divided into 4 groups, high, medium, and low dose groups and negative control groups, 20 each. The negative control group was given distilled water, and the test subjects were given 0.25g/(kg.d), 0.50g/(kg.d), and 1.50g/(kg.d) of 3 doses (corresponding to 5, 10, and 30 times of the recommended intake amount in humans, and the doses were low dose group, medium dose group, and high dose group, respectively). The test sample was administered for 30 days.
The evaluation indexes are established and gavage is carried out for 1 time every day for 30 days continuously, animals are fasted for 24 hours before dissection, and the experiment is carried out on the 31 th day according to the test method for enhancing the immunity function in the health food functional evaluation program and test method specification issued by the ministry of health. The animals were gazed for 1 hour before challenge with antigen to immunize the mice. And (4) continuously performing evaluation on each index after the intragastric administration for 4 days, wherein the cellular immune function, the humoral immune function, the monocyte-macrophage function and the NK cell activity are taken as evaluation indexes.
Data processing and result determination
1.5.1 statistical treatment significance of data differences between groups the statistical treatment of one-way anova was performed using SPSS16.0 statistical software, with P < 0.05 as the difference being significant.
Results in the determination of four aspects of cell immune function, humoral immune function, monocyte-macrophage function and NK cell activity, the results of a mouse delayed type allergic reaction experiment, serum hemolysin determination and a mouse abdominal cavity macrophage phagocytosis fluorescent microsphere experiment are all positive, and the success of the experiment and the reliability of an experiment system are shown by the statistical significance (P < 0.05) of the difference through the analysis of single-factor variance. The high and medium dose groups set in the experiment have significant difference with the control group, the immune function has the trend of enhancement, and the difference has statistical significance.
The function evaluation experiment shows that the dispersible tablet sample produced according to the invention has the function of enhancing immunity.
The scope of the present invention should not be considered limited to the particular embodiments and examples described above. It will be clear to a person skilled in the art that several simple deductions or equivalent substitutions can be made without departing from the basic idea of the invention, which equivalent alternatives are still to be considered within the scope of protection of the invention.

Claims (2)

1. The ginseng fritillaria ussuriensis health food is characterized by being prepared from the following raw materials in parts by weight: 4 parts of ginseng and 3 parts of fritillary bulb;
the health food is a preparation prepared by taking an extract of fritillaria ussuriensis, fine ginseng powder, a ginseng water extract and a ginseng alcohol extract as active ingredients and adding auxiliary materials acceptable for health food;
the preparation of the health food comprises the following components: granules, capsules and tablets;
the preparation method of the health food comprises the following steps: firstly, preparing raw materials; pulverizing Ginseng radix; extracting fritillary bulb; extracting the ginseng; fifthly, collecting paste; preparing a soft material; granulating and finishing granules; eighthly, forming;
the preparation method of the health food is characterized by comprising the following steps:
(1) weighing ginseng according to the formula, crushing and sieving, wherein ginseng fine powder passes through a 120-mesh sieve, and ginseng coarse powder which does not pass through the 120-mesh sieve are reserved;
(2) weighing fritillary bulb according to the formula, extracting for 2 times by using 40-90% ethanol as a solvent according to the material-liquid ratio of 1:10 and 1:8 respectively for 2 hours and 1 hour, filtering, and combining the filtrates to obtain an extract I for later use;
(3) extracting the ginseng coarse powder for 2 times at room temperature by adopting an ultrasonic circulation method, wherein the interval ultrasonic ratio is 0.6s:0.5 s-0.6 s:4.5s, the power is 300-700W, water is used as a solvent for the first time, the material-liquid ratio is 1: 10-1: 12, the extraction time is 0.5 h-1.5 h, the extracted material liquid is centrifuged, the supernatant is filtered, and the filtrate is collected to obtain an extracting solution II for later use; taking 60-85% ethanol as a solvent for the second time, taking the material-liquid ratio as 1:8, extracting for 0.5h, centrifuging the extracted material liquid, taking supernatant, filtering, and collecting filtrate to obtain an extracting solution III for later use;
(4) mixing the extract I and the extract II, concentrating under reduced pressure, drying at low temperature, and pulverizing to obtain extract powder, or spray drying to obtain extract powder;
(5) mixing Ginseng radix fine powder, adjuvant and extract powder, adding extractive solution III as binder, and kneading to obtain soft material;
(6) placing the soft material in a granulator, granulating to obtain wet granules, boiling and drying the wet granules, and finishing granules after drying to obtain dry granules;
(7) filling the dry granules into an aluminum-plastic packaging bag to obtain granules; filling into empty capsule to obtain capsule; tabletting in a tabletting machine to obtain the tablet.
2. Use of the health food according to claim 1 in health foods for contributing to enhancement of immune function.
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CN104073416A (en) * 2014-07-10 2014-10-01 朱长怀 Ginseng health liquor and preparation method thereof
CN104872680A (en) * 2015-06-25 2015-09-02 绿之韵生物工程集团有限公司 Healthcare food composition capable of boosting immunity
CN105521256A (en) * 2016-02-23 2016-04-27 延边大学 Ranae oviductus and fritillariae ussuriensis bulbus soft capsule as well as preparation method and applications thereof
CN105533749A (en) * 2016-02-19 2016-05-04 延边大学 Health food containing herba epimedii and fructus schizandrae and preparing method and application thereof

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Publication number Priority date Publication date Assignee Title
CN104073416A (en) * 2014-07-10 2014-10-01 朱长怀 Ginseng health liquor and preparation method thereof
CN104872680A (en) * 2015-06-25 2015-09-02 绿之韵生物工程集团有限公司 Healthcare food composition capable of boosting immunity
CN105533749A (en) * 2016-02-19 2016-05-04 延边大学 Health food containing herba epimedii and fructus schizandrae and preparing method and application thereof
CN105521256A (en) * 2016-02-23 2016-04-27 延边大学 Ranae oviductus and fritillariae ussuriensis bulbus soft capsule as well as preparation method and applications thereof

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