Ginseng donkey-hide gelatin paste and preparation method thereof and method of quality control
Technical field
The present invention relates to herbal paste technical fields, in particular to a kind of ginseng donkey-hide gelatin paste and preparation method thereof and quality
Control method.
Background technique
Herbal paste also known as paste are run after fame with its dosage form, are belonged to ball in Chinese medicine, are dissipated, eight kinds of cream, pellet, wine, dew, soup, ingot agent
One of type.The meaning of cream is wider: such as finger object, using grease as cream;Such as finger-type state, with solidifying without solid title cream;Refer to taste, such as with sweet ginger
Sliding fat is cream.The Classic of Mountains and Rivers was said in once: " it is cream that speech taste is well all sliding ", such as finger content is acted on the essence for object, such as finger, to grow
Cream profit is supported as length.Oral pastes are widely used for the sections such as inside and outside, woman, youngster, the injury of the bone, eye ear mouth and nose because it plays tonic effect
Illness and big person physically weak after being ill.It is on the basis of large-scale compound decoction, according to the different constitutions of people, different clinical manifestations
Different prescriptions are established, mix certain auxiliary materials after dense decoct and a kind of manufactured stiff shape is semi-fluid or freeze shape dosage form.Wherein, prescription
Middle drug is used as much as possible authentic medicinal herbs, and whole manufacturing process operations are stringent, only the final ability of the herbal paste Jing Guo retrofit
As top grade.
As people's rhythm of life is increasingly accelerated, the appearance of many sub-health populations is caused, cardinal symptom shows as losing
Sleep, is irritated, vulnerable etc., also easily there is such symptom in the middle-aged and the old and climacteric women.Therefore a kind of science conjunction is provided
Reason, the health invigorant beneficial to health are even more important.
Herbal paste food currently on the market is various in style, and product quality is irregular, many with product made from ginseng, point
It is also not many with product made from dendrobium candidum, donkey-hide gelatin, but there is not yet the cream prepared with ginseng, donkey-hide gelatin, dendrobium candidum science
Slurry product appears on the market.103238844 A of CN discloses a kind of ginseng donkey-hide gelatin paste and preparation method thereof, with ginseng, Poria cocos, fructus lycii, Ah
Glue, dark plum, yam and red dates, orange peel, fructus amomi are raw material, and soaking, decoction, concentration, allotment, cooling, filling, sterilizing, packaging are made
, preparation process is coarse, and ginseng is unprocessed, and nutriment is lost seriously, and lotion quality does not control.
It is therefore desired to seek the new significant herbal paste product of safe, steady, at a specified future date health-care effect.
In view of this, the present invention is specifically proposed.
Summary of the invention
One of the objects of the present invention is to provide a kind of ginseng donkey-hide gelatin paste, it is formulated rationally science, uses 50~500nm of partial size
Ultra micro dusting ginseng, can increase the dissolution rate and bioavilability of ginseng, enhance pharmacological action, herbal paste delicate mouthfeel temperature
Profit, sugariness are suitable for having effects that fill blood, supporting taste, beneficial lung kidney tonifying, antitoxic heart-soothing and sedative.
The second object of the present invention is to provide a kind of preparation method of above-mentioned ginseng donkey-hide gelatin paste, using herbal paste technique, respectively
Active constituent is retained well in raw material, is suitable for industrialized production.
The third object of the present invention is to provide a kind of method of quality control of above-mentioned ginseng donkey-hide gelatin paste, preferably controls and be somebody's turn to do
The quality of product, can effectively work under supervision, be more advantageous to the control of product quality, guarantee the stabilization of product quality, food clothes
With safer.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
In a first aspect, providing a kind of ginseng donkey-hide gelatin paste, mainly it is prepared by the raw material of following parts by weight: partial size 50~
5~50 parts of 1~100 part of 12.5~25 parts of 5~25 parts of ginseng submicron powder, donkey-hide gelatin, rhizoma polygonati, the dendrobium candidum of 500nm, fructus lycii 0~
100 parts, 0~50 part of Siraitia grosvenorii, 0~100 part of Saussurea involucrata culture, 0~100 part of jujube, 0~100 part of Semen sesami nigrum, sweetener 0~
100 parts and water.
Preferably, on the basis of technical solution provided by the invention, ginseng donkey-hide gelatin paste is mainly by the original of following parts by weight
Material is prepared: 1~100 part of 12.5~25 parts of 5~25 parts of ginseng submicron powder, donkey-hide gelatin, rhizoma polygonati, the iron sheet of 50~500nm of partial size
It is 5~50 parts of dendrobium nobile, 20~100 parts of fructus lycii, 20~50 parts of Siraitia grosvenorii, 20~100 parts of Saussurea involucrata culture, 10~100 parts of jujube, black
10~100 parts of sesame, 10~100 parts of sweetener and water.
Preferably, on the basis of technical solution provided by the invention, ginseng donkey-hide gelatin paste is mainly by the original of following parts by weight
Material is prepared: 50~100 parts of 20~25 parts of 10~25 parts of ginseng submicron powder, donkey-hide gelatin, rhizoma polygonati, the iron sheet of 50~500nm of partial size
It is 30~50 parts of dendrobium nobile, 50~60 parts of fructus lycii, 50~60 parts of Siraitia grosvenorii, 40~60 parts of Saussurea involucrata culture, 50~100 parts of jujube, black
50~100 parts of sesame, 30~80 parts of sweetener and water.
Preferably, on the basis of technical solution provided by the invention, the ginseng submicron powder of the 50~500nm of partial size
Preparation method the following steps are included:
(a) pretreated ginseng is subjected to cryogenic freezing, and low-temperature grinding, obtains the ginseng coarse powder of 40~100 mesh;
(b) ginseng coarse powder is subjected to low-temperature vacuum microwave drying, and low temperature supersonic jet mill is obtained to 50~500nm
To ginseng submicron powder;Or ginseng coarse powder is subjected to co-vibration mill crushing, obtain the ginseng submicron powder of 50~500nm.
Preferably, on the basis of technical solution provided by the invention, in step (a), the temperature of cryogenic freezing is -20~
0 DEG C, preferably -20~-5 DEG C;
Preferably, in step (a), the temperature of low-temperature grinding is -5~10 DEG C, preferably -5~5 DEG C.
Preferably, on the basis of technical solution provided by the invention, in step (b), the dry work of low-temperature vacuum microwave
Skill condition includes: microwave power: 4~6kW, drying temperature be -5~0 DEG C, drying time be 1~2h, vacuum degree be 0.04~
0.06Pa;
Preferably, in step (b), the temperature of low temperature supersonic jet mill is -5~10 DEG C, preferably -5~5 DEG C;
Preferably, in step (b), the temperature that co-vibration mill crushes is at 20 DEG C hereinafter, it is preferred that 0~20 DEG C.
Second aspect provides a kind of preparation method of above-mentioned ginseng donkey-hide gelatin paste, comprising the following steps:
(a) rhizoma polygonati, dendrobium candidum, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum are added
Water is decocted, and takes decoction liquor to be concentrated after decoction, obtains concentrate;
(b) by concentrate, dissolve after donkey-hide gelatin, sweetener and be tuned into the ginseng submicron powder of paste, the training of optional saussurea involucrata
Feeding object is deployed, and ginseng donkey-hide gelatin paste is obtained.
Preferably, on the basis of technical solution provided by the invention, the preparation method of ginseng donkey-hide gelatin paste includes following step
It is rapid:
(a) rhizoma polygonati, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum is taken to soak in water 30
~40min;
(b) rhizoma polygonati after immersion, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum are added
Enter and decocted in 8~12 times of amount water twice, separation merges decoction liquor, and decoction liquor is concentrated under reduced pressure into relative density 1.10~1.30, obtains
To concentrate A;
(c) fritter dendrobium candidum is added in 8~12 times of amount water and is decocted twice, separation merges decoction liquor, decoction liquor decompression
It is concentrated into relative density 1.10~1.30, obtains concentrate B;
(d) heating in 1~2 times of amount water and 1~2 times of amount yellow rice wine is added in donkey-hide gelatin dissolves donkey-hide gelatin completely;Sweetener is molten
Change;Donkey-hide gelatin after dissolving is merged with sweetener, and is concentrated into relative density 1.10~1.30, obtains concentrate C;
(e) ultra micro dusting ginseng and optional Saussurea involucrata culture are tuned into paste with water, obtain paste D;
(f) concentrate A, concentrate B, concentrate C and paste D are deployed, continues to be concentrated into relative density 1.25
~1.40, obtain ginseng donkey-hide gelatin paste.
One of the third aspect provides a kind of method of quality control of above-mentioned ginseng donkey-hide gelatin paste, include the following steps
Or several combination:
(I) ginseng identifies: using ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 as reference substance, thin-layer chromatography
In, test sample at the position corresponding to the chromatogram of the reference substance, shows the spot of same color;
(II) donkey-hide gelatin identifies: using glycine, proline, alanine, L- hydroxyproline as reference substance, in thin-layer chromatography,
Test sample at the position corresponding to the chromatogram of the reference substance, shows the spot of same color;
(III) fructus lycii identifies: using fructus lycii as control medicinal material, in thin-layer chromatography, test sample is corresponding to reference medicine chromatography
Position on, show same color spot;
(IV) relative density determination: 20 DEG C must not be less than 1.25;
(V) in terms of glucan, 2.0g/100g must not Thick many candies assay: be less than containing Thick many candies;
(VI) total saponin content measures: in terms of ginsenoside Re, must not be less than 300mg/100g containing total saposins.
Preferably, on the basis of technical solution provided by the invention, in step (I), test sample is lotion successively through three
What chloromethanes and n-butanol ultrasonic extraction obtained;The solvent that thin-layer chromatography uses is chloroform-methanol-water solution, colour developing
Agent is ethanol solution of sulfuric acid;
Preferably, in step (II), test sample is that lotion is extracted at 105 DEG C through hydrochloric acid and obtained;Thin-layer chromatography uses
Solvent be phenol-borax-aqueous solution, color developing agent is ethanol solution of ninhydrin;
Preferably, in step (III), test sample is that lotion extracts to obtain through ethyl acetate;The expansion that thin-layer chromatography uses
Agent is ethyl acetate-chloroform-formic acid solution, sets and develops the color under ultraviolet light.
Compared with the prior art, the invention has the following beneficial effects:
(1) the raw materials used in the present invention ginseng uses the ginseng submicron powder of 50~500nm of partial size, can increase the dissolution of ginseng
Rate and bioavilability save the dosage of ginseng, retain the volatile active of ginseng, enhance pharmacological action, and table is compared in raising
Area improves dispersing uniformity, improves and absorbs, improves mouthfeel.
(2) herbal paste of the present invention includes a variety of nourishing famous-objects such as ginseng, donkey-hide gelatin, dendrobium candidum, by raw material scientific compatibility, sufficiently
The complementary coordinative role of paste nourishing agent is played, body is grown and moistens body, the normal phase takes to have and fills blood, supports taste, beneficial lung kidney tonifying, antitoxic heart-soothing and sedative
The effect of, resistance, anti-aging, beautifying face and moistering lotion can be improved.
(3) present invention can preferably control the quality of kind by method of quality control, and effectively work under supervision more has
Conducive to the control of product quality, guarantee the stabilization of product quality, food is taken safer.
(4) preparation process of the present invention retains the active constituent in raw material well, is suitable for industrialized production.
(5) the raw materials used present invention is dual-purpose of drug and food articles as defined in health ministry, and any food additive is not used
Add agent, it is edible safety, without any side effects.
Detailed description of the invention
Fig. 1 is the photo of ginseng donkey-hide gelatin paste made from one embodiment of the present invention;
Fig. 2 is the thin-layer chromatogram of ginseng under daylight;
Fig. 3 is the thin-layer chromatogram of fructus lycii under ultraviolet light;
Fig. 4 is the thin-layer chromatogram of donkey-hide gelatin under daylight.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
According to an aspect of the invention, there is provided a kind of ginseng donkey-hide gelatin paste, is mainly prepared by the raw material of following parts by weight
It obtains: 1~100 part of 12.5~25 parts of 5~25 parts of ginseng submicron powder, donkey-hide gelatin, the rhizoma polygonati of 50~500nm of partial size, dendrobium candidum 5~
50 parts, 0~100 part of fructus lycii, 0~50 part of Siraitia grosvenorii, 0~100 part of Saussurea involucrata culture, 0~100 part of jujube, Semen sesami nigrum 0~100
Part, 0~100 part of sweetener and water.
Ginseng is herbaceos perennial, contains ginsenoside, panaxan, panacene's alcohols, the poly- second of ginseng in ginseng
The various actives substance such as acetylenic, volatile oil can adjust central nervous system, promote utilization of the brain to energy matter, change
Kind cardiac function, reduces blood glucose, enhances body's immunity.In addition, ginseng also has antitumor and oxidation resistant function.At present
In the market there are many ginseng product, these ginseng products are mostly to be made by extracting active constituent from ginseng, still
Ginseng active constituent contains fat-soluble and water-soluble two substance simultaneously, and existing extracting method cannot soak simultaneously Multiple components
Out, a kind of active material can only be targetedly extracted, the waste of ginseng active constituent is caused.If using traditional processing side
Method, will be directly edible after ginseng boiling, enriches ingredient although remaining the active material of ginseng whole, contained by ginseng and is not easy
For human body digestion and absorption, the medical tonic effect of ginseng cannot be given full play to comprehensively, so that the bioavilability of ginseng is lower.This
Outside, the sterilization technology in existing processing of Panax ginseng method easily makes ginseng rotten, and room temperature one month or so just usually in air
It will appear discoloration, spoiled phenomenon.
The present invention uses ginseng submicron powder, is that ginseng obtains after pulverizing, partial size, can be effective in 50~500nm
The activity for keeping ginseng functional component, significantly improves the dissolution and absorption of wherein effective component, gives full play to ginseng effect.
The typical but non-limiting parts by weight of ginseng submicron powder are, for example, 5 parts, 10 parts, 15 parts, 20 parts or 25 parts.
Donkey-hide gelatin, it is sweet in flavor mild-natured, return liver, lung, kidney channel, have tonify the blood and arrest bleeding, the function of nourishing Yin and moistening lung.Donkey-hide gelatin contain gelatin it is former,
With various trace elements, a variety of amino acid etc., these are all the important substances of human nutrition for ossein, protein, are had obvious anti-ageing
Always, promote longevity effect, donkey-hide gelatin can improve the phagocytic activity of macrophage, have effects that improve immunity, the calcium in donkey-hide gelatin
Content is higher, can increase the intake of internal calcium after taking, and bone calcium caused by being effectively improved because of calcium deficiency is lost, and donkey-hide gelatin, which has, to be improved
Red blood cell number and amount of hemoglobin, the effect for promoting hemopoietic system to restore can increase blood leukocytes in raying organism, red
Cell quantity and content of hemoglobin reduce damage of the ray to biological somatic stem cell, and donkey-hide gelatin also can increase body freedom
The expression of base scavenger enzyme reduces destruction of the free radical to hemopoietic system, to play radiation protection.
The typical but non-limiting parts by weight of donkey-hide gelatin are, for example, 12.5 parts, 15 parts, 17.5 parts, 20 parts, 22.5 parts or 25
Part.
Rhizoma polygonati, it is sweet in flavor, it is mild-natured, it is nontoxic, there is boosting qi and nourishing yin, invigorating the spleen, moistening lung, the function of kidney-nourishing.
The typical but non-limiting parts by weight of rhizoma polygonati are, for example, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts, 50 parts, 60
Part, 70 parts, 80 parts, 90 parts or 100 parts.
Dendrobium candidum is orchid family Dendrobium Sw, is one of the orchid recorded earliest in China's ancient documents.Dendrobium nobile
Type, the whole world just have more than 1500 kinds, and there are about 76 kinds in China.Dendrobium candidum is wherein the most rare, medical value highest one
A kind, Shennong's Herbal are classified as top grade, it is indicated that dendrobium candidum has the function of promote the production of body fluid, quench the thirst, easing pain, eliminating oedema
Effect, cures mainly the diseases such as the pyreticosis deficiency of Yin, mesh are dark, stomach is weak, hoarseness, to vocal cords fatigue, hoarseness, restore its U.S. sound have it is special
Curative effect.The main component of dendrobium candidum includes polysaccharide, alkaloid, stilbenes compound, sesquiterpenoids, phenolic acid, lignanoids etc..Iron
The polysaccharide component of skin dendrobium nobile can promote humoral immunity of organism, cellular immune function and induce cytokine profiles, have enhancing
The effect of immunity of organisms, stilbenes compound then have apparent antitumor action.Dendrobium candidum tissue culture has relatively strong
Scavenger of ROS ability, by significantly improve superoxide dismutase (SOD) level, reduce lipid peroxide (LPO) make
With finally removing interior free yl.Dendrobium candidum also has the effects that antifatigue, hypoglycemic, eliminating phlegm and relieving cough, in malignant tumour
Adjuvant treatment, chronic gastritis, diabetes, chronic pharyngitis, weakness due to chronic disease immunologic hypofunction, eye health etc. have extensively
Application.
The typical but non-limiting parts by weight of dendrobium candidum are, for example, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts or 50 parts.
Fructus lycii (fructus lycii) is optional raw material, and fructus lycii is sweet in flavor mild-natured, and function is nourshing kidney, moistening lung, tonifying liver, improving eyesight.
The typical but non-limiting parts by weight of fructus lycii are, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts, 50
Part, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts.
Siraitia grosvenorii is optional raw material, and Siraitia grosvenorii contains the medicinal ingredients such as mogroside, a variety of amino acid and vitamin, sieve
Its contained Momordica-Glycosides of Chinese fruit does not generate heat than 300 times of sucrose sweet tea, is the rare raw material of beverage, confectionery industry, is sucrose
Best substitute.Often drink " Luohan " fruit tea, can prevent a variety of diseases.
The typical but non-limiting parts by weight of Siraitia grosvenorii be, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts or
50 parts.
Saussurea involucrata culture is optional raw material, and Saussurea involucrata culture is compositae plant Saussurea laniceps flower (SaussureaLaniceps
Hand.-Mazz.), snow lotus of big bud flower also known as Saussurea involucrata (Saussureainvolucrata Kar.et Kin), jellyfish snow
The wounded in the battle complete stool of lotus flower (Saussurea medusa Maxim) etc. is the active constituent that raw material extracts.Lanatechead saussurea herb with flower is warm-natured, sweet in flavor
The benefits of hardship returns liver,spleen,kidney three to pass through, and tool is except cold, establishing-Yang, menstruation regulating, hemostasis, the ingredient isolated is extracted from saussurea involucrata mainly Huang
Ketone, Coumarins, Anthraquinones and sesquiterpenoids etc. have anti-inflammatory and antalgic, antitumor, Antiradiation injury, antioxygen
The effects of change, terminal pregnancy, also there is certain effect to cardiovascular system.
The typical but non-limiting parts by weight of Saussurea involucrata culture are, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40
Part, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts.
Jujube is optional raw material also known as jujube, for being dried to for Rhamnaceae plant jujube (Ziziphusjujuba Mill.)
Ripe fruit.Its is sweet in flavor, warm-natured.Returns spleen, stomach, the heart channel of Hang-Shaoyin, there is the benefits of tonifying middle-Jiao and Qi, nourishing blood and tranquilization.
The typical but non-limiting parts by weight of jujube are, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts, 50
Part, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts.
Semen sesami nigrum is optional raw material, original name flax, for being dried to for Pedaliaceae plant sesame (Sesamumindicum L.)
Ripe seed.Its is sweet in flavor, mild-natured.Return liver, kidney, large intestine channel.With nourishing liver and kidney, benefiting essence-blood, the dry effect of ease constipation.Semen sesami nigrum contains greatly
The fat and protein of amount, also containing nutritional ingredients such as carbohydrate, VitAVitE, lecithin, calcium, iron, chromium.Semen sesami nigrum
There is stomach invigorating, liver protection, strengthen immunity, promote red blood cell growth, while internal melanin can be increased, is conducive to hair
Growth.
The typical but non-limiting parts by weight of Semen sesami nigrum are, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts,
50 parts, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts.
Sweetener is optional raw material, and typical but non-limiting sweetener is, for example, carbohydrate, such as rock sugar, xylitol etc..
The typical but non-limiting parts by weight of sweetener are, for example, 0 part, 1 part, 5 parts, 10 parts, 20 parts, 30 parts, 40 parts,
50 parts, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts.
Ginseng donkey-hide gelatin paste of the present invention " mainly by ... " means it in addition to the raw material, can also include other raw materials.It removes
It is " mainly by ... " of the present invention except this, it may be replaced by enclosed " for " or " by ... ".
The ginseng submicron powder that 50~500nm of partial size is used in raw material of the present invention, can increase the dissolution rate and biology of ginseng
Availability saves the dosage of ginseng, retains the volatile active of ginseng, enhances pharmacological action, and increasing specific surface area improves
Dispersing uniformity improves and absorbs, improves mouthfeel.The present invention is organically combined using ginseng submicron powder, dendrobium candidum and donkey-hide gelatin, rhizoma polygonati
Ginseng donkey-hide gelatin paste is made, ginseng, dendrobium candidum, which are entered donkey-hide gelatin, can play distinctive health-care effect, raw using the tonifying Qi of ginseng
Saliva, tranquilize the mind and promote the intelligence and other effects, the strong healthcare function of the sweet Wen Zhirun of donkey-hide gelatin, blood tonification effect, while dendrobium candidum reinforcing stomach reg fluid is utilized,
The ginseng donkey-hide gelatin food of good health and a long life is developed in nourishing Yin and clearing heat and other effects.The formula of the invention is reasonable, science, herbal paste delicate mouthfeel
Gentle, sugariness is suitable for having the effect of filling blood, support taste, beneficial lung kidney tonifying, antitoxic heart-soothing and sedative, both to deficiency-cold in spleen and stomach, do not think to drink
Food, anaemia, vulnerable, dysphoric people have good opsonic action, and to the big person of pressure, the middle-aged and the old and climacteric woman
The subhealth symptom that female is easy to appear has good prevention effect, is the good merchantable brand in nourishing food.
Preferably, ginseng donkey-hide gelatin paste is mainly prepared by the raw material of following parts by weight: the ginseng of 50~500nm of partial size is super
5~25 parts of micro mist, 12.5~25 parts of donkey-hide gelatin, 1~100 part of rhizoma polygonati, 5~50 parts of dendrobium candidum, 20~100 parts of fructus lycii, Siraitia grosvenorii
20~50 parts, 20~100 parts of Saussurea involucrata culture, 10~100 parts of jujube, 10~100 parts of Semen sesami nigrum, 10~100 parts of sweetener and
Water.
It is further preferred that ginseng donkey-hide gelatin paste is mainly prepared by the raw material of following parts by weight: 50~500nm's of partial size
10~25 parts of ginseng submicron powder, 20~25 parts of donkey-hide gelatin, 50~100 parts of rhizoma polygonati, 30~50 parts of dendrobium candidum, 50~60 parts of fructus lycii,
50~60 parts of Siraitia grosvenorii, 40~60 parts of Saussurea involucrata culture, 50~100 parts of jujube, 50~100 parts of Semen sesami nigrum, sweetener 30~80
Part and water.
By optimizing compatibility, and fructus lycii, Siraitia grosvenorii, Saussurea involucrata culture, jujube, Semen sesami nigrum being added etc. it to each raw material
His raw material, can obtain the herbal paste of tonic better effect.
In a preferred embodiment, the preparation method of the ginseng submicron powder of 50~500nm of partial size includes following step
It is rapid:
(a) pretreated ginseng is subjected to cryogenic freezing, and low-temperature grinding, obtains the ginseng coarse powder of 40~100 mesh;
(b) ginseng coarse powder is subjected to low-temperature vacuum microwave drying, and low temperature supersonic jet mill is obtained to 50~500nm
To ginseng submicron powder;Or ginseng coarse powder is subjected to co-vibration mill crushing, obtain the ginseng submicron powder of 50~500nm.
Preferably, in step (a), pretreatment includes: to take fresh ginseng medicinal material, removes impurity, is eluted with water, it is cut into 2~
4cm sections;Preferably, the temperature of cryogenic freezing is -20~0 DEG C, preferably -20~-5 DEG C, such as -20 DEG C, -15 DEG C, -10 DEG C, -5
DEG C or 0 DEG C;Preferably, the temperature of low-temperature grinding is -5~10 DEG C, preferably -5~5 DEG C, such as -5 DEG C, 0 DEG C, 2 DEG C, 5 DEG C or 10
℃。
Preferably, in step (b), the dry process conditions of low-temperature vacuum microwave include: microwave power: 4~6kW, such as
4kW, 5kW or 6kW;Drying temperature is -5~0 DEG C, such as -5 DEG C, -2 DEG C, -1 DEG C or 0 DEG C;Drying time is 1~2h, such as
1h, 1.5h or 2h;Vacuum degree is 0.04~0.06Pa, such as 0.04Pa, 0.05Pa or 0.06Pa.
Interval 30s can be taken in microwave drying process, heating the microwave treatment mode of 30s, (i.e. every heating 30s just stops
Then heating 30s is further continued for heating 30s stops heating 30s again, circuits sequentially.
Preferably, the temperature of low temperature supersonic jet mill is -5~10 DEG C, preferably -5~5 DEG C, such as -5 DEG C, 0 DEG C, 2
DEG C, 5 DEG C or 10 DEG C.
Preferably, in step (b), the temperature that co-vibration mill crushes at 20 DEG C hereinafter, it is preferred that 0~20 DEG C, such as 0 DEG C, 5 DEG C,
10 DEG C, 15 DEG C or 20 DEG C.Its partial size is set to reach 50~500nm after crushing, the detection of partial size can pass through scanning electron microscope, laser
The methods of particle size analyzer is detected.
Preferably, it is dispensed and is packed after step (b), comprising: smashed ginseng submicron powder is taken, through power 1kW, frequency
At 18~26 DEG C of temperature after microwave sterilization 2min under conditions of rate 2450MHz, the aseptic subpackaged room below of humidity 65% is according to every
The specification of packet 500g is dispensed, and ginseng submicron powder is made.
Through ginseng submicron powder made from low temperature three times different grinding modes, the work of ginseng functional component can be more effectively kept
Property, the dissolution and absorption of wherein effective component are significantly improved, ginseng efficacy exertion is more abundant.
According to the second aspect of the invention, a kind of preparation method of above-mentioned ginseng donkey-hide gelatin paste, including following step are provided
It is rapid:
(a) rhizoma polygonati, dendrobium candidum, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum are added
Water is decocted, and takes decoction liquor to be concentrated after decoction, obtains concentrate;
(b) by concentrate, dissolve after donkey-hide gelatin, sweetener and be tuned into the ginseng submicron powder of paste, the training of optional saussurea involucrata
Feeding object is deployed, and ginseng donkey-hide gelatin paste is obtained.
Preparation process of the present invention retains the active constituent in raw material well, is suitable for industrialized production.
Preferably, a kind of preparation method of typical ginseng donkey-hide gelatin paste the following steps are included:
(a) rhizoma polygonati, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum is taken to soak in water 30
~40min;
(b) rhizoma polygonati after immersion, optional fructus lycii, optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum are added
Enter and decocted in 8~12 times of amount water twice, separation merges decoction liquor, and decoction liquor is concentrated under reduced pressure into relative density 1.10~1.30, obtains
To concentrate A;
(c) fritter dendrobium candidum is added in 8~12 times of amount water and is decocted twice, separation merges decoction liquor, decoction liquor decompression
It is concentrated into relative density 1.10~1.30, obtains concentrate B;
(d) heating in 1~2 times of amount water and 1~2 times of amount yellow rice wine is added in donkey-hide gelatin dissolves donkey-hide gelatin completely;Sweetener is molten
Change;Donkey-hide gelatin after dissolving is merged with sweetener, and is concentrated into relative density 1.10~1.30, obtains concentrate C;
(e) ultra micro dusting ginseng and optional Saussurea involucrata culture are tuned into paste with water, obtain paste D;
(f) concentrate A, concentrate B, concentrate C and paste D are deployed, continues to be concentrated into relative density 1.25
~1.40, obtain ginseng donkey-hide gelatin paste.
Preferably, 8~12 times of amount water refer to that it is rhizoma polygonati, optional fructus lycii, optional sieve that the weight of water, which is added, in step (b)
Chinese fruit, 8~12 times of optional jujube and optional Semen sesami nigrum total amount.Step (b) specifically includes: by rhizoma polygonati, optional fructus lycii,
It is boiled in optional Siraitia grosvenorii, optional jujube and optional Semen sesami nigrum and 8~12 times of amount pure water investment jacketed pans, Yu Jia
It is passed through the biggish steam of flow in the interlayer of layer pot, turns steam flow down after boiling, keeps 1~2h of slight boiling condition, stops adding
Heat, the stainless mesh screen net filtration of 80~200 mesh, filtrate are stored in storage tank;It is pure that 8~12 times of amounts of the above raw material gross weight are added into filter residue
Water, with for the first time, filtering, merging filtrate stands 6~10h, takes supernatant, subtracted with inspissator decocting method in above-mentioned storage tank
Pressure is concentrated into relative density 1.10~1.30.
Preferably, 8~12 times of amount water refer to that the weight that water is added is 8~12 times of dendrobium candidum weight in step (c).Step
Suddenly (c) is specifically included: by dendrobium candidum or fresh dendrobium candidum, cutting adds and is endured in 8~12 times of amount pure water investment jacketed pans
System turns steam flow down in being passed through the biggish steam of flow in the interlayer of jacketed pan after boiling, and keeps 1~2h of slight boiling condition,
Stop heating, the stainless mesh screen net filtration of 80~200 mesh, filtrate is stored in storage tank;The above raw material gross weight 8~12 is added into filter residue
Amount pure water again, decocting method is with for the first time, and filtering, for merging filtrate in above-mentioned storage tank, 6~10h of standing takes supernatant, use is dense
Contracting device is concentrated under reduced pressure into relative density 1.10~1.30.
Preferably, step (d) specifically includes: taking donkey-hide gelatin, the water of 2 times of its amount and the heating of 1 times of yellow rice wine is added to keep donkey-hide gelatin complete
It dissolves, filters;Rock sugar is taken, a small amount of sodium citrate is added to dissolve with appropriate pure water, is filtered;Donkey-hide gelatin after dissolving is merged with rock sugar,
And it is concentrated into relative density 1.10~1.30.
Yellow rice wine is made using rice, milled glutinous broomcorn millet, grain by raw material, belongs to low brewed wine, contains 21 kinds of amino acid, which includes
Several unknown amino acids, and human body itself cannot synthesize and must all have by 8 kinds of essential amino acid yellow rice wine of food intake, yellow rice wine
Promoting blood circulation, tying-in network function, yellow rice wine enters liver kidney, mutually must be used with donkey-hide gelatin, the effect of donkey-hide gelatin skin maintenance and cosmetic benefits tonifying Qi is performed to
It is best.
Preferably, after step (f) further include: the bottle cleaned up is taken, by the filling concentrated extract of specified amount, is sealed, bar
30~90min of family name's sterilizing, cooling, packaging.
According to the third aspect of the present invention, a kind of method of quality control of above-mentioned ginseng donkey-hide gelatin paste is provided, including with
The combination of one or more of lower step:
(I) ginseng identifies: using ginsenoside Rb1, ginsenoside Re and ginsenoside Rg1 as reference substance, thin-layer chromatography
In, test sample shows the spot of same color on the corresponding position of reference substance chromatography;
(II) donkey-hide gelatin identifies: using glycine, proline, alanine, L- hydroxyproline as reference substance, in thin-layer chromatography,
Test sample at the position corresponding to the chromatogram of the reference substance, shows the spot of same color;
(III) fructus lycii identifies: using fructus lycii as control medicinal material, in thin-layer chromatography, test sample is corresponding to reference medicine chromatography
Position on, show same color spot;
(IV) relative density determination: 20 DEG C must not be less than 1.25;
(V) in terms of glucan, 2.0g/100g must not Thick many candies assay: be less than containing Thick many candies;
(VI) total saponin content measures: in terms of ginsenoside Re, must not be less than 300mg/100g containing total saposins.
Relative density refers under identical temperature, pressure condition, the ratio between density and the density of water of substance.Except as otherwise rule
Fixed outer, temperature is 20 DEG C.
Relative density determination can be according to Chinese Pharmacopoeia 0601 method of version general rule in 2015.
Thick many candies assay can edit the survey of Thick many candies in " health food functional component detection method " according to Wang Guangya
Determine method spectrophotometry.
Total saponin content measurement can be according to " in health food total in " health food examine with assessment technique specification " 2003 editions
The measurement of saponin(e ".
Preferably, step (I) specifically includes: take cream body 2.5g, adds chloroform 20ml, is ultrasonically treated 10min, filters,
The dregs of a decoction are spare, volatilize chloroform, and residue adds water 0.5ml stirring wet, adds water saturated n-butanol 20ml, is ultrasonically treated
30min divides and takes n-butanol liquid, washed 2 times with 3 times of amount ammonia solutions, discard cleaning solution, n-butanol liquid is evaporated, and residue adds methanol lml
Make to dissolve, as test solution.Separately take ginsenoside Rb1's reference substance, ginsenoside Re's reference substance and ginsenoside Rg1's control
Product add methanol that every lml is made respectively containing the solution of lmg, as reference substance solution.According to thin-layered chromatography (Chinese Pharmacopoeia version in 2015
One general rule 0502) test, above-mentioned each 2 μ l of four kinds of solution is drawn, is put respectively on same silica gel g thin-layer plate, with chloroform-
10 DEG C of methanol-water (13:7:2) lower layer's solution arranged below is solvent, is unfolded, and takes out, dries, and is sprayed with 10% sulfuric acid ethyl alcohol
It is clear to be heated to spot development at 105 DEG C for solution.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show identical
The spot of color.
Preferably, step (II) specifically includes: take cream body lg is set in tool plug test tube, adds 6mol/L hydrochloric acid solution 4ml, close
Plug, sets in 105 DEG C of baking ovens and heats 6 hours, add water 6ml, shake up, and filters, and filtrate is evaporated, and it is molten that residue adds 10% ethyl alcohol 10ml to make
Solution, as test solution.Glycine reference substance, L- hydroxyproline reference substance separately are taken, adds 10% ethyl alcohol that every lml is made and contains
The mixed solution of lmg, as reference substance solution.It is tested according to thin-layered chromatography (one general rule 0502 of Chinese Pharmacopoeia version in 2015),
2 μ l of test solution, 1 μ l of reference substance solution are drawn, is put respectively in making into ribbon on same silica gel g thin-layer plate, with phenol-
0.5% borax soln (4:1) is solvent, is unfolded, and takes out, dries, and spray is heated with 0.2% ethanol solution of ninhydrin at 105 DEG C
It is clear to spot development.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown.
Preferably, step (III) specifically includes: take cream body 10g adds water 20ml, shakes up, and heating is boiled 15 minutes, let cool,
Filtration, filtrate are shaken with ethyl acetate 15ml and are extracted 2 times, and each 20ml, combined extract is evaporated, and residue adds ethyl acetate 1ml
Make to dissolve, as test solution.Fructus lycii control medicinal material 1g separately is taken, is made in the same way of control medicinal material solution.According to thin-layered chromatography
(one general rule 0502 of Chinese Pharmacopoeia version in 2015) test, draws each 10 μ l of above two solution, puts respectively thin in same silica G
On laminate, to be ethyl acetate-chloroform-formic acid (3:2:1) for solvent, it is unfolded, takes out, dry, set ultraviolet lamp
It is inspected under (365nm);In sample chromatogram, on position corresponding with reference medicine chromatography, the fluorescence spot of same color is shown.
The present invention can preferably control the quality of kind by method of quality control, can effectively work under supervision, more have
Conducive to the control of product quality, guarantee the stabilization of product quality, food is taken safer.
It elaborates combined with specific embodiments below with comparative example to the present invention.
Embodiment 1
A kind of preparation method of ginseng submicron powder, comprising the following steps:
1) it pre-processes: taking fresh ginseng medicinal material, remove impurity, be eluted with water, be cut into 2~4cm sections;
2) cryogenic freezing: the ginseng section that step 1) obtains being spread out and is freezed, and cryogenic temperature is -20 DEG C;
3) low-temperature grinding: the ginseng section that step 2) obtains is crushed under 5 DEG C of cryogenic conditions, is sieved, obtain 40~
The coarse powder of 100 mesh;
4) low-temperature vacuum microwave is dry: the ginseng coarse powder that step 3) is obtained carries out low-temperature vacuum microwave drying, opens electricity
Source adjusts microwave power: 6kW, the microwave drying time: 1h, drying temperature: 0 DEG C, vacuum degree: 0.06Pa;In microwave drying process
Every heating 30s just stops heating 30s and then being further continued for heating 30s stopping heating 30s again, circuits sequentially;
5) low temperature supersonic jet mill: the ginseng xeraphium that step 4) obtains is surpassed under 0 DEG C of cryogenic conditions
Crushing of Ultrafine, reaching its partial size between 50~500nm, (detection of its partial size passes through the side such as scanning electron microscope, laser particle analyzer
Method is detected);
6) packing and packaging: taking ginseng submicron powder made from step 5), micro- under conditions of frequency 2450MHz through power 1kw
Wave sterilize 2min after at 20 DEG C of temperature, the aseptic subpackaged room below of humidity 65% is dispensed, according to it is every packet 500 grams specification into
Row packing, is made ginseng submicron powder.
Embodiment 2
A kind of preparation method of ginseng submicron powder, comprising the following steps:
1) it pre-processes: taking fresh ginseng medicinal material, remove impurity, be eluted with water, be cut into 2~4cm sections;
2) cryogenic freezing: the ginseng section that step 1) obtains being spread out and is freezed, and cryogenic temperature is -5 DEG C;
3) low-temperature grinding: the ginseng section that step 2) obtains is crushed under 0 DEG C of cryogenic conditions, is sieved, obtain 40~
The coarse powder of 100 mesh;
4) low-temperature vacuum microwave is dry: the ginseng coarse powder that step 3) is obtained carries out low-temperature vacuum microwave drying, opens electricity
Source adjusts microwave power: 4kW, the microwave drying time: 1.5h, drying temperature: -5 DEG C, vacuum degree: 0.04Pa;Microwave drying
Every heating 30s just stops heating 30s and then being further continued for heating 30s stopping heating 30s again in journey, circuits sequentially;
5) co-vibration mill crushes: the ginseng coarse powder that step 4) obtains being carried out nanometer pulverization in co-vibration mill, temperature control exists
20 DEG C hereinafter, reaching its partial size between 50~500nm, (detection of its partial size passes through scanning electron microscope, laser particle analyzer etc.
Method is detected);
6) packing and packaging: taking ginseng submicron powder made from step 5), micro- under conditions of frequency 2450MHz through power 1kw
Wave sterilize 2min after at 25 DEG C of temperature, the aseptic subpackaged room below of humidity 65% is dispensed, according to it is every packet 500 grams specification into
Row packing, is made ginseng submicron powder.
Embodiment 3
A kind of ginseng donkey-hide gelatin paste, raw material include: the ginseng submicron powder 25g, donkey-hide gelatin 25g, rhizoma polygonati 100g, iron sheet of embodiment 1
Dendrobium nobile 50g and sweetener 50g.
Embodiment 4
Embodiment 4-12 the difference is that raw material and content are different, the raw material of embodiment 4-12 and contains from embodiment 3
Amount is as shown in table 1.
Table 1
Embodiment 13
The present embodiment and the difference of embodiment 3 are that ginseng submicron powder is purchased from Ningxia Kai Yuan Bioisystech Co., Ltd.
Embodiment 14-24
Prepare ginseng donkey-hide gelatin paste according to the formula of embodiment 3-13, preparation method the following steps are included:
1) rhizoma polygonati, fructus lycii, Siraitia grosvenorii, jujube, Semen sesami nigrum are taken, is soaked in water 30~40 minutes;
2) by 8 times of rhizoma polygonati, fructus lycii, Siraitia grosvenorii, jujube, Semen sesami nigrum and above-mentioned raw materials total amount amount pure water investment folders after immersion
It is boiled in layer pot, in being passed through the biggish steam of flow in the interlayer of jacketed pan, turns steam flow down after boiling, keep micro-
Boiling state 2 hours, stop heating, the stainless mesh screen net filtration of 80~200 mesh, filtrate is stored in storage tank;More than being added into filter residue
8 times of amount pure water of raw material gross weight, with for the first time, filtering, merging filtrate standing 8 hours or more, takes decocting method in above-mentioned storage tank
Supernatant is concentrated under reduced pressure into relative density 1.20 with inspissator;
3) donkey-hide gelatin is taken, adds the water of 2 times of its amount and the heating of 1 times of yellow rice wine to dissolve donkey-hide gelatin completely, filters;Sweetener is taken, is added
A small amount of sodium citrate is dissolved with appropriate pure water, is filtered;Donkey-hide gelatin after dissolving is merged with sweetener, and is concentrated into relative density
1.10;
4) ginseng submicron powder and Saussurea involucrata culture are taken, is tuned into paste with appropriate pure water;
5) by fresh dendrobium candidum, cutting adds and is boiled in its 10 times amount pure water investment jacketed pans, in the folder of jacketed pan
It is passed through the biggish steam of flow in layer, turns steam flow down after boiling, is kept for slight boiling condition 1 hour, heating, 100 mesh are stopped
Stainless mesh screen net filtration, filtrate are stored in storage tank;It is added 10 times of amount pure water of the above raw material gross weight into filter residue, decocting method is the same as the
Once, it filters, merging filtrate stands 8 hours, take supernatant, be concentrated under reduced pressure into relative density with inspissator in above-mentioned storage tank
1.10~1.30;
6) it 3), 4), 5) will merge to be added in 2) and continue to be concentrated into lotion relative density 1.35, obtain concentrated extract;
7) bottle cleaned up is taken, by the filling concentrated extract of specified amount, sealing, pasteurization or 121 DEG C of steam sterilizings
30min, cooling, packaging.
Comparative example 1
The difference of this comparative example and embodiment 3 is, replaces dendrobium candidum with the sweetener of equivalent.Preparation method is the same as implementation
Example 3.
Comparative example 2
The difference of this comparative example and embodiment 3 is, replaces rhizoma polygonati with the sweetener of equivalent.Preparation method is the same as embodiment 3.
Comparative example 3
The difference of this comparative example and embodiment 3 is, replaces dendrobium candidum and rhizoma polygonati with the sweetener of equivalent.Preparation method
With embodiment 3.
Comparative example 4
The difference of this comparative example and embodiment 3 is, replaces ginseng submicron powder with ginseng.People is participated in rhizoma polygonati by preparation method
It decocts together.
Comparative example 5
A kind of ginseng donkey-hide gelatin paste, raw material include: ginseng submicron powder 2g, donkey-hide gelatin 50g, rhizoma polygonati 100g, the iron sheet stone of embodiment 1
Dry measure used in former times 3g and sweetener 95g.
Test example 1
For verifying effect of the invention, crowd's test-meal test has been carried out:
1, crowd is tested
Test carries out in the street square return of spring Tang Hefang shop, and choosing 750 has the mid-aged population of deficiency of vital energy deficiency of blood symptom to be tried
Test observation.
2, test method
Embodiment 14-24 and comparative example the 1-4 ginseng donkey-hide gelatin paste being prepared are supplied to test crowd to take.It will examination
The crowd of testing is divided into 15 groups, and every group of 50 people take the ginseng donkey-hide gelatin paste that embodiment 14-24 and comparative example 1-4 are prepared respectively.
3, test period
Test period is the last week in Winter Solstice, total to take 60 days to after the beginning of spring.
4, instructions of taking
Subject daily 2 times, 1 spoon (about 20~30g), is taken after mixing it with water every time with boiled water.
5, testing standard
Effective: sleep state is obviously improved, and has appetite, is had rosy cheeks, and dizzy fatiguability out of strength is obviously improved;
Effective: sleep state makes moderate progress, and loss of appetite makes moderate progress, sallow complexion or it is pale make moderate progress, it is dizzy weary
Power fatiguability makes moderate progress.
Efficient=(effective+effectively)/total number of cases × 100%;Obvious effective rate=effective/total number of cases × 100%.
6, test result
It takes after expiring, statistical results, as shown in table 2.
Table 2
Group |
Test number |
Effective number |
Efficiently individual quantity |
Obvious effective rate |
It is efficient |
Embodiment 14 |
50 |
44 |
6 |
88% |
100% |
Embodiment 15 |
50 |
46 |
4 |
92% |
100% |
Embodiment 16 |
50 |
45 |
5 |
90% |
100% |
Embodiment 17 |
50 |
48 |
2 |
96% |
100% |
Embodiment 18 |
50 |
49 |
1 |
98% |
100% |
Embodiment 19 |
50 |
48 |
2 |
96% |
100% |
Embodiment 20 |
50 |
47 |
3 |
94% |
100% |
Embodiment 21 |
50 |
49 |
1 |
98% |
100% |
Embodiment 22 |
50 |
49 |
1 |
98% |
100% |
Embodiment 23 |
50 |
50 |
0 |
100% |
100% |
Embodiment 24 |
50 |
40 |
9 |
80% |
98% |
Comparative example 1 |
50 |
38 |
8 |
76% |
92% |
Comparative example 2 |
50 |
40 |
9 |
80% |
98% |
Comparative example 3 |
50 |
35 |
12 |
70% |
94% |
Comparative example 4 |
50 |
36 |
11 |
72% |
94% |
Comparative example 5 |
50 |
40 |
8 |
80% |
96% |
Table 2 as can be seen that ginseng donkey-hide gelatin paste of the invention have fill blood well, support taste, beneficial lung kidney tonifying, calming heart are pacified
Effect of mind has good opsonic action to deficiency-cold in spleen and stomach, do not feel like eating, anaemia, vulnerable, dysphoric people, is one
The nourishing top grade of kind effectively, safe.
Embodiment 17-23 is on the basis of embodiment 14, as fructus lycii, Siraitia grosvenorii, jujube, Semen sesami nigrum and saussurea involucrata are cultivated
The addition of the ingredients such as object can further promote the effect of enhancing herbal paste, achieve significant nourishing regulating effect.
The effect of embodiment 14 is more preferable compared with embodiment 24, it is seen that the ginseng submicron powder being prepared using breaking method three times
More commercially available ginseng submicron powder effect is more preferable.
Comparative example 1-3 lacks rhizoma polygonati and/or dendrobium candidum, and 5 ginseng submicron powder of comparative example, donkey-hide gelatin and dendrobium candidum proportion are not
Together, the curative effect of ginseng donkey-hide gelatin paste reduces, it is seen then that herbal paste is obtained by ginseng submicron powder, the reasonable compatibility of dendrobium candidum and donkey-hide gelatin
Curative effect good ginseng donkey-hide gelatin paste.
Comparative example 4 does not use ginseng submicron powder, and ginseng donkey-hide gelatin paste curative effect obtained is substantially reduced, this is because using partial size
The ginseng submicron powder of 50~500nm can increase the dissolution rate and bioavilability of ginseng, enhance ginseng pharmacological action, improve
It absorbs.
Fig. 1 is the photo of ginseng donkey-hide gelatin paste made from one embodiment of the present invention, measures Thick many candies 2.1g/100g, total
Saponin(e 0.76g/100g.
Embodiment 25
A kind of ginseng donkey-hide gelatin paste method of quality control, comprising:
(1) ginseng identifies: take cream body 2.5g adds chloroform 20ml, is ultrasonically treated 10 minutes, and filtration, the dregs of a decoction are spare, wave
Dry chloroform, residue add water 0.5ml stirring wet, add water saturated n-butanol 20ml, be ultrasonically treated 30 minutes, divide and take positive fourth
Alcohol liquid is washed 2 times with 3 times of amount ammonia solutions, discards cleaning solution, n-butanol liquid is evaporated, and residue adds methanol lml to make to dissolve, as confession
Test sample solution.Ginsenoside Rb1's reference substance, ginsenoside Re's reference substance and ginsenoside Rg1's reference substance separately are taken, methanol is added to be made
Every lml is respectively containing the solution of lmg, as reference substance solution.According to thin-layered chromatography (one general rule 0502 of Chinese Pharmacopoeia version in 2015)
Above-mentioned each 2 μ l of four kinds of solution is drawn in test, is put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (13:7:
2) 10 DEG C of lower layer's solution arranged below are solvent, are unfolded, and take out, dry, and are sprayed with 10% ethanol solution of sulfuric acid, at 105 DEG C
It is clear to be heated to spot development.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown;
(2) donkey-hide gelatin identifies: taking this product lg, sets in tool plug test tube, add 6mol/L hydrochloric acid solution 4ml, close plug sets 105 DEG C of bakings
It is heated 6 hours in case, adds water 6ml, shake up, filtered, filtrate is evaporated, and residue adds 10% ethyl alcohol 10ml to make to dissolve, as test sample
Solution.Glycine reference substance, proline, alanine, L- hydroxyproline reference substance separately are taken, adds 10% ethyl alcohol that every lml is made and contains
The mixed solution of lmg, as reference substance solution.It is tested according to thin-layered chromatography (one general rule 0502 of Chinese Pharmacopoeia version in 2015),
2 μ l of test solution, 1 μ l of reference substance solution are drawn, is put respectively in making into ribbon on same silica gel g thin-layer plate, with phenol-
0.5% borax soln (4:1) is solvent, is unfolded, and takes out, dries, and spray is heated with 0.2% ethanol solution of ninhydrin at 105 DEG C
It is clear to spot development.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown;
(3) 1.25 (Chinese Pharmacopoeia version general rules 0601 in 2015) must not (20 DEG C) of relative density measurements: be less than.
Embodiment 26
A kind of ginseng donkey-hide gelatin paste method of quality control, comprising:
(1) ginseng identifies: add chloroform 20ml, is ultrasonically treated 10 minutes, filtration, the dregs of a decoction are spare, and chloroform is volatilized,
Residue adds water 0.5ml stirring wet, adds water saturated n-butanol 20ml, is ultrasonically treated 30 minutes, divides and takes n-butanol liquid, with 3 times
It measures ammonia solution to wash 2 times, discards cleaning solution, n-butanol liquid is evaporated, and residue adds methanol lml to make to dissolve, as test solution.Separately
Ginsenoside Rb1's reference substance, ginsenoside Re's reference substance and ginsenoside Rg1's reference substance are taken, adds methanol that every lml is made and contains
The solution of lmg, as reference substance solution.It tests, draws according to thin-layered chromatography (one general rule 0502 of Chinese Pharmacopoeia version in 2015)
Above-mentioned each 2 μ l of four kinds of solution, puts respectively on same silica gel g thin-layer plate, with 10 DEG C of chloroform-methanol-water (13:7:2) with
Lower layer's solution of lower placement is solvent, is unfolded, and takes out, dries, and sprays with 10% ethanol solution of sulfuric acid, is heated to spot at 105 DEG C
Point colour developing is clear.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown;
(2) fructus lycii identifies: taking this product 10g, adds water 20ml, shake up, heating is boiled 15 minutes, is let cool, is filtered, and filtrate is used
Ethyl acetate 15ml shaking is extracted 2 times, and each 20ml, combined extract is evaporated, and residue adds ethyl acetate 1ml to make to dissolve, as
Test solution.Fructus lycii control medicinal material 1g separately is taken, is made in the same way of control medicinal material solution.According to thin-layered chromatography (Chinese Pharmacopoeia
One general rule 0502 of version in 2015) test, each 10 μ l of above two solution is drawn, is put respectively on same silica gel g thin-layer plate, with
It is ethyl acetate-chloroform-formic acid (3:2:1) for solvent, expansion takes out, dries, set and examine under ultraviolet lamp (365nm)
Depending on;In sample chromatogram, on position corresponding with reference medicine chromatography, the fluorescence spot of same color is shown;
(3) 1.25 (Chinese Pharmacopoeia version general rules 0601 in 2015) must not (20 DEG C) of relative density measurements: be less than.
Embodiment 27
A kind of ginseng donkey-hide gelatin paste method of quality control, comprising:
(1) donkey-hide gelatin identifies: take cream body lg is set in tool plug test tube, adds 6mol/L hydrochloric acid solution 4ml, and close plug sets 105 DEG C of bakings
It is heated 6 hours in case, adds water 6ml, shake up, filtered, filtrate is evaporated, and residue adds 10% ethyl alcohol 10ml to make to dissolve, as test sample
Solution.Glycine reference substance, proline, alanine, L- hydroxyproline reference substance separately are taken, adds 10% ethyl alcohol that every lml is made and contains
The mixed solution of lmg, as reference substance solution.It is tested according to thin-layered chromatography (one general rule 0502 of Chinese Pharmacopoeia version in 2015),
2 μ l of test solution, 1 μ l of reference substance solution are drawn, is put respectively in making into ribbon on same silica gel g thin-layer plate, with phenol-
0.5% borax soln (4:1) is solvent, is unfolded, and takes out, dries, and spray is heated with 0.2% ethanol solution of ninhydrin at 105 DEG C
It is clear to spot development.In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown;
(2) 2.0g/100g must not Thick many candies assay: be less than containing Thick many candies (in terms of glucan).Standard glucose is molten
Liquid: 0.1g is accurately weighed by 105 DEG C of dry glucose to constant weight, 100mL is diluted to water after being dissolved in water, this solution
1mL glucose containing 1mg, used time therefrom draw 10mL, are settled to 250mL with distilled water, the concentration note of this glucose standards solution
For C (about 40 μ g/mL or so).The preparation of standard curve: precision pipette glucose standards solution 0.4,0.6,0.8,1.0,1.2,
1.4,1.6mL is respectively mended with water to 2.0mL, even with rotation vortex mixer vibration, and 6% phenol 1.0mL is then added, uses swirl mixing device
Shake even, then plus the 5mL concentrated sulfuric acid, shake rapidly even.It is placed at room temperature for 5min, 15min is then kept the temperature in boiling water bath, it is cooling with tap water
5min, then with rotation vortex mixer vibration it is even, at 490nm wavelength measure OD value, using 2.0mL water by same color operation as
Blank is that ordinate draws standard curve with glucose standards solution volume number (ml) using OD value as abscissa.For
The preparation of solution: take cream body 1g is tried, sets in test tube plus distilled water 45mL, ultrasonic dissolution is centrifuged after being cooled to room temperature, collect
Supernatant is settled to 100mL (being denoted as V1, Unit/mL).Above-mentioned filtered fluid 1.0mL is accurately drawn, is placed in 10mL centrifuge tube, adds
Enter dehydrated alcohol 4mL, after mixing, 4 DEG C of standing 6h, centrifugation discards supernatant liquid.80% (V/V) ethyl alcohol number milliliter rinse of residue,
It is buckled on filter paper, operates 3~4 times repeatedly.Residue is sufficiently dissolved with water, can suitably be heated (60 DEG C of <, be cooled to room temperature), and
Constant volume is to 50mL (being denoted as V2, Unit/mL).Pipette samples liquid 1.0mL (being denoted as V3, Unit/mL) (is equivalent to the more of 40 μ g or so
Sugar makes optical density OD survey the optimum range more than 0.2~0.6, increases and decreases the absorption of sample liquid as one sees fit if polysaccharide amount is too high or too low
Amount, but must not exceed 2mL, need to increase the sample amount of weighing if being more than, that is, increase the amount of weighing of m), add water to be supplemented to
2.00mL, it is even with rotation vortex mixer vibration, 6% phenol solution 1.0mL is then added, it is even with rotation vortex mixer vibration, then plus the dense sulphur of 5mL
Acid shakes rapidly even.It is placed at room temperature for 5min, 15min is then kept the temperature in boiling water bath, cools down 5min with tap water, then mixed with rotation
Even device vibration is even, measures optical density (OD survey) at wavelength 490nm.It is surveyed according to OD and standard curve checks in V3 and is equivalent to glucose mark
The volume number V4 of quasi- solution, Unit/mL.Calculate to get.Method foundation: Wang Guangya edits " health food functional component detection side
Method " in Thick many candies measuring method spectrophotometry), make an amendment;
(3) total saponin content measures: containing total saposins in terms of ginsenoside Re, must not be less than 300mg/100g.Sample pretreating:
The sample (being accurate to 0.001g) for weighing 5g or so is transferred in 100mL volumetric flask with hot water dissolving, adds 60mL water, ultrasound
Then 30min is settled to 100mL with water, shake up, and places, and Aspirate supernatant 0.5mL carries out column chromatography.Column chromatography: it is infused with 10mL
Emitter makees chromatographic column, and built-in 3cm Amberlite-XAD-2 macroreticular resin, above plus 1cm neutral alumina first uses 25mL70% second
Alcohol washes column, discards eluent, then wash column with 25mL, discards eluent, accurate to be added on the processed sample solution of 0.5mL
Column discards eluent with the washing column of 25mL to wash away the water-solubility impurities such as sugared part, with 25mL70% ethanol elution saponin(e, receives
Collect eluent in evaporating dish, the bath that discharges water volatilizes.It is used as colour developing with this.Colour developing: accurately add in the above-mentioned evaporating dish volatilized
Enter 0.2mL5% vanillic aldehyde glacial acetic acid solution, rotate evaporating dish, dissolve residue all, then plus 0.8mL perchloric acid, moved into after mixing
In 5mL band plug graduated glass pipe, it is placed in 60 DEG C of water-baths and heats 10min, take out, after the molten cooling of ice, glacial acetic acid is accurately added
5.0mL, after shaking up, to carry out colorimetric estimation together with standard pipe at 1cm colorimetric pool hand 560nm wavelength.Standard pipe: ginseng is drawn
Saponin(e Re standard solution (2.0mg/mL: accurately weighs ginsenoside Re standard items 0.020g, is dissolved and be settled to methanol
10.0mL, i.e. every milliliter of 2.0mg containing ginsenoside Re) 100 μ L are added in 10mL test tube, are placed on water-bath and volatilize (lower than 60 DEG C),
Or hot blast drying (not making to overheat), it is operated from " 3 colour developings: accurate that 0.2mL5% vanillic aldehyde glacial acetic acid solution ... is added " below,
It is identical as sample.Measure absorbance value.Calculate to get.Method foundation: referring to " health food is examined and assessment technique specification "
In 2003 editions " measurements of total saposins in health food ".
Fig. 2 be daylight under ginseng thin-layer chromatogram, wherein 1,2 be test sample, 3 be ginsenoside Rb1's reference substance, 4
It is ginsenoside Rg1's reference substance for ginsenoside Re's reference substance, 5;Fig. 3 is the thin-layer chromatogram of fructus lycii under ultraviolet light 365nm,
Wherein 1,3 be test sample, and 2,4 be fructus lycii control medicinal material;Fig. 4 is the thin-layer chromatogram of donkey-hide gelatin under daylight, wherein 1 is 2 μ L
Test sample, 2 be 1 μ L test sample, and 3 be glycine, and 4 be proline, and 5 be alanine, and 6 be L- hydroxyproline.
By being controlled using the above method of quality control, the quality of kind can be preferably controlled, is effectively supervised
Production, is more advantageous to the supervision of product quality, guarantees the stabilization of product quality, food is taken safer.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.