CN108042709A - A kind of steamed sealwort concocting method - Google Patents
A kind of steamed sealwort concocting method Download PDFInfo
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- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8969—Polygonatum (Solomon's seal)
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Abstract
The invention discloses a kind of steamed sealwort concocting methods, comprise the following steps:It by fresh sealwort removal impurity and fibrous root, cleans and dries 12 36h, be placed in 30 50 DEG C of baking ovens, dry 12 36h make its moisture reach 25 40%;5 10mm of sheet is cut in taking-up, and then dry 12 36h in 40 DEG C of baking ovens, make its moisture reach 15 24%;Dried sealwort section, is placed in and steams in container, steam 4 8h, take out;55 80 DEG C of 10 20h of heated-air drying make its moisture reach 12 15% and steam a solarization sealwort to get one;It repeats above operation four times and steams five solarization sealworts to get five;Five steamings, five solarization sealworts, which are placed in, to be steamed in container, is steamed 4 8h, is taken out;70 80 DEG C of heated-air dryings make moisture reach 7% and steam six solarization sealworts to get six;5 HMF contents of product >=0.6mg/g.Concocting method optimization design of the present invention is steamed in clear soup technique working process stage by stage, and sealwort product quality is more preferably outstanding, and mouthfeel, natural component content have significant healthcare applications advantage better than the prior art.
Description
Technical field
The present invention relates to a kind of steamed sealwort concocting methods, belong to Chinese medicine processing technique field.
Background technology
Sealwort, Huangjing, POLYGONATI RHIZOMA are that liliaceous plant this product is liliaceous plant P. kingianum
Polygonatum kingianum Coll.et Hemsl., sealwort Polygonatum sibiricum Red. or David's-harp
The dry rhizome of Polygonatum cyrtonema Hua.It is different by shape, it practises and claims " big sealwort ", " polygonatum sibiricum Redoute ", " ginger shape
Sealwort ".
【Nature and flavor and channel tropism】Sweet and neutral.Returns spleen, lung, kidney channel.
【Function is with curing mainly】Boosting qi and nourishing yin, invigorating the spleen, moistening lung, kidney-nourishing.For deficiency of spleen-QI and stomach-QI, fatigue and asthenia, deficiency of stomach-Yin, mouth
Xerophagia is few, deficiency syndrome of the lung cough caused by dryness, overstrain cough hemoptysis, asthenia of essence and blood, soreness and weakness of waist and knees, poliosis, Heat Diabetes.
Modern medical experiment research shows that sealwort has anti-aging, adjusts immunity, cardiac stimulant, anticancer, raising and improve note
Recall a variety of effects such as power, the Natural Medicine Chemistry ingredient contained by sealwort includes:Polysaccharide, oligosaccharide, steroid saponin, alkaloid,
Amino acid, trace element etc..
Raw sealwort has numb taste, and throat can be stimulated by directly taking, and dispute is numb, contacts directly raw sealwort or sealwort juice meeting
Cause pruitus.Therefore picking obtained fresh sealwort needs, by processing, to eliminate its irritation side effect, ability is preferably
Using.
Existing sealwort processing procedure includes medicine materical crude slice, stir-baked RHIZOMA POLYGONATI with yellow rice wine etc..States Pharmacopoeia specifications:Sealwort decoction piece is that sealwort is removed impurity,
It cleans, slightly moistens, cut sheet, dry gained finished product;Stir-baked RHIZOMA POLYGONATI with yellow rice wine is to clean sealwort, according to wine stew method or wine steam method stew or steam it is saturating,
It slightly dries in the air, cuts sheet, it is dry.The processing procedure of existing sealwort is shallower for the processing depth of sealwort, is eliminated for sealwort side effect
And natural effective component release action is relatively limited in sealwort.
On the one hand the processing characteristic of sealwort decoction piece and stir-baked RHIZOMA POLYGONATI with yellow rice wine makes its application range be limited to traditional practical application more and mends
Gas yin-nourishing, invigorating the spleen, moistening lung, effect, which remains, exploits potentialities;On the other hand traditional concocting method limits sealwort to a certain extent
Edible health is worth, convenient property, and it is still necessary to further improve for eating mouth feel etc..
The content of the invention
It is an object of the invention to the sealwort tradition processing procedure in the presence of the prior art is overcome to limit sealwort application
Deficiency provides a kind of steamed sealwort concocting method and steamed sealwort quality detecting method.
In order to realize foregoing invention purpose, the present invention provides following technical schemes:
A kind of steamed sealwort concocting method, comprises the following steps:
(1) by fresh sealwort removal impurity and fibrous root, clean and dry 12-36h, be placed in 30-50 DEG C of baking oven, it is dry
12-36h makes its moisture reach 25-40%, and sheet 5-10mm is cut in taking-up, and then the dry 12-36h in 40 DEG C of baking ovens, makes
Its moisture reaches 15-24%.
(2) the dried sealwort of step 1 is cut into slices, is placed in and steams in container, steam 4-8h, taken out.55-80 DEG C of hot air drying
Dry, dry 10-20h makes its moisture reach 12-18% and steams a solarization sealwort to get one.
(3) repeat above step 2 and operate four times to get five steamings, five solarization sealworts.
Five solarization sealworts of (4) five steaming, which are placed in, to be steamed in container, is steamed 4-8h, is taken out.70-80 DEG C of heated-air drying, makes moisture
Reach 7% and steam six solarization sealworts to get six.
Obtained six, which steam six, shines in sealwort, 5-HMF contents >=0.6mg/g.
Compared with common sealwort decoction piece, stir-baked RHIZOMA POLYGONATI with yellow rice wine, sealwort is carried out with States Pharmacopoeia specifications for the present invention steamed sealwort concocting method
Steamed processing so that sealwort is more preferably outstanding as the mouthfeel that health products are eaten, and appearance is easy for consumers to accept, promotes its health products food
Convenience.Six are steamed by six simultaneously and shine the steamed sealwort of processing, improve polysaccharide, 5-HMF, diosgenin in steamed sealwort
Content promotes the Natural Medicine Chemistry component content of sealwort, enhances health-care efficacy so that the health value higher of sealwort is more prominent
Go out.5-HMF (5 hydroxymethyl furfural) content in particularly steamed sealwort is higher, by controlling 5-HMF levels effective
Ensure effect/quality grade that steamed sealwort processes.5-HMF directly reacts steamed sealwort by glucose or fructose dehydration generation
The level of processing is studied by inventor and found when the control of 5-HMF contents levels is in more than 0.6mg/g in steamed sealwort
It waits, sealwort quality is more outstanding, meets the demand of health products practical application value maximization.
Meanwhile processing procedure of the present invention control six steams six and shines sealwort moistures below 7%, be the instruction of processing degree with
And the external manifestation of the damaed cordition of active ingredient, moisture in steamed sealwort is controlled so that the steamed sealwort quality of finished product is excellent
Show has good storage stability, can preferably maintain its stability for a long time, avoids steamed sealwort after steamed process
Nutrient enriches deficiency apt to deteriorate.Finally, steamed sealwort is prepared by concocting method of the present invention, gained sealwort finished product, which moistens, to be had
Gloss, soft texture;Section cutin, sepia;Periphery brownish black gas is micro-, sweet, and that chews has stickiness.Existing sealwort is overcome to process
The sealwort decoction piece of technique preparation, stir-baked RHIZOMA POLYGONATI with yellow rice wine are not preferably the defects of ordinary consumer is eaten as health products, add Siberian solomonseal rhizome health-care
Effect is worth, it is easier to be chosen for ordinary consumer edible.
Further, step 1, clean and dry 20-26h, be placed in 38-45 DEG C of baking oven, dry 15-26h makes its moisture
Reach 25-35%.Preferably, step 1, clean and dry, be placed in 38-43 DEG C of baking oven, dry 20-26h reaches its moisture
To 25-32%.
Further, step 1, take out by dry sealwort, cut 7-9mm sheets, it is then dry in 35-45 DEG C of baking oven
12-30h makes its moisture reach 17-24%.Preferably, step 1, take out by dry sealwort, cut 7-8mm sheets, so
The dry 12-28h in 36-43 DEG C of baking oven afterwards, makes its moisture reach 18-20%.
It on the clean sealwort dried in step 1 carries out that processing is pre-dried, which is divided into the progress of two steps, first
Processing is dried before being section so that its moisture tentatively reduces, followed by drying process causes again after section
Moisture further reduces.By drying twice, the particularly front and rear drying process independent twice of section delays plant cell
Slow dehydration, it is uniform to not only contribute to section, and be conducive to polyoses content be unlikely to reduce in this step it is too fast, after being more advantageous to
Mucilaginous removal in sealwort during face steams.By accurately controlling fresh sealwort that processing, slicing processing is pre-dried
The speed that middle moisture is sloughed realizes the drying effect needed for design, is to ensure that necessity of steamed sealwort final products quality
Condition.
It is pre-dried especially by above-mentioned preferred fresh sealwort, slicing treatment technique, the overall quality of sealwort is significantly
Degree is promoted, and has significance.
Further, the steamed sealwort that prepared by concocting method of the present invention is used as food, beverage, alternative tea and health food etc..
The steamed sealwort processing procedure method of the present invention, which fully steams in clear soup sealwort, to be handled so that and the quality of sealwort is significantly promoted,
Further, step 1, sealwort slice thickness 5-9mm, it is preferable that slice thickness 6-8mm.
Further, during sealwort steams, 3 times steam and steamed in clear soup using big fire, latter 3 times clear using slow boiling progress
It steams, steams in total 6 times.
Preferably, during big fire is steamed in clear soup, vapor (steam) temperature >=100 DEG C in container are steamed.
Preferably, during slow boiling is steamed in clear soup, 98-100 DEG C of vapor (steam) temperature in container is steamed.
Further, step 2, the section of dried sealwort, which is placed in, steams in container, steams 5-7h, then 57-65 DEG C of hot air drying
Dry, dry 12-18h makes its moisture reach 12-18% and steams a solarization sealwort to get one.
Further, in step 2-3, after steaming sealwort each time, the dry degree for making the reduction of its moisture gradually rises,
Dry sealwort moisture reaches 12-18% after steaming for the first time, and dry sealwort moisture is less than for the first time after steaming for the second time, and the 3rd
It is secondary less than second, less than third time, be less than the 4th time for the 5th time for the 4th time.Dry sealwort moisture is extremely after steaming for 5th time
7-12%.The ingredients such as colloid, cell liquid, glue matter are gradually steamed and released in sealwort when steaming each time, are passed through
It continuously steams, drying process, realizes the more preferable removing for side effect ingredient in sealwort, for polysaccharide, 5-HMF, Chinese yam soap
The conversion or release of the ingredients such as aglycon.
Further, step 4, five steamings, five solarization sealworts are placed in and steamed in container, steamed 5-7h, take out, 72-78 DEG C of heated-air drying
20-28h makes its moisture reach less than 7% and steams six solarization sealworts to get six.Step 4 is to realize that final six steam six and shine sealwort
The technical process of processing, processing procedure of the present invention pass through in the process not each time by sealwort drying to moisture 7%
Repeatedly slowly steamed, drying process, particularly last time drying process drying temperature are slightly above front drying process several times, do
Dry degree is stronger.When sealwort is by preamble repeatedly steamed and drying process, purified major part has steamed needs to remove in the process
Ingredient, last time fully drying is conducive to finally the steam in clear soup drying of sealwort and product drying extent control.In this way
Gradually incremental processing state modulator so that the cell of sealwort root tuber is slowly dehydrated, and is effectively removed mucilaginous substance in sealwort, to the greatest extent may be used
Other polysaccharide constituents can be retained.
Further, step 4, in the sealwort processed, Determination of Diosgenin >=1.5%.It is examined using HPLC chromatogram method
The steamed Determination of Diosgenin in Rhizoma polygonati of analysis is surveyed, determines that steamed sealwort reaches expected product by analyzing Determination of Diosgenin
Matter grade is worth with more outstanding health-care efficacy.Although with someone in the prior art by the way of the total Dioscin of test
The quality grade of the steamed sealwort of evaluation, total Dioscin is one kind of total steroidal saponin, has antitumor, the cardiovascular work(of improvement
The effect of immunity, platelet aggregation-against can, be adjusted, but the quality of total Dioscin reaction sealwort is more fuzzy, is directed to
Ingredient it is numerous, it is impossible to the effective steamed sealwort of difference processes front and rear difference, is imitated for the differentiation of processing procedure quality grade
Fruit is bad.
Further, step 4, the sealwort processed, water-soluble extractives content >=50%.According to《Chinese Pharmacopoeia》2015
Version the 4th (general rule 2201) is tested, and using hot dipping, is measured by solvent of water.Water-soluble extractives is that reaction sealwort is clear
It steams after processing, processes important 0 index of degree, the sealwort water-soluble extractives content fully processed is high, easily impregnates release
Effective component can either maximize as health products or pharmaceutical applications and play effect meaning.Suitable water-soluble leaching
Object content ratio is conducive to be promoted mouthfeel when steamed sealwort is eaten as health products and nutritional ingredient is easy to absorb application
Ratio.
Further, step 4, in the sealwort processed, polyoses content >=4%.Determination of polysaccharide, containing Siberian solomonseal rhizome polysaccharide with
DEXTROSE ANHYDROUS (C6H12O6) meter.The steamed Polysaccharide in Polygonatum sibiricum of the present invention is not highest sealwort product, but the present invention exists
The steamed sealwort optimization of control steams technical process so that diosgenin and water-soluble extractives content are effectively controlled, phase
The steamed Polysaccharide in Polygonatum sibiricum answered becomes more suitable.Polysaccharide is too unfavorable for the mouthfeel of steamed sealwort and carries instead in sealwort
It rises, passes through the steamed process of the present invention, on the basis of diosgenin and water-soluble extractives is controlled, corresponding polysaccharide
Component content might not highest, but suitable Determination of Diosgenin and polyoses content so that sealwort mouthfeel is more preferably pure, clear
It is cool so that steamed sealwort product is more preferable as the effect that health products are applied, and is worth higher.
Preferably, using ultraviolet-uisible spectrophotometer Polysaccharide in Polygonatum sibiricum is tested in 485-495nm wave-length coverages.
The polyoses content tested using ultraviolet-uisible spectrophotometer in sealwort has the characteristics that implementation simple to operation, and polysaccharide exists
There is maximum absorption band at 485nm, testing precision is preferable.
Preferably, sealwort sample is steamed in clear soup using ethyl alcohol heating and refluxing extraction, and ethanol extract is divided light using UV, visible light
Degree measurement examination polyoses content.
Further, step 4, sealwort moisture≤7% processed.It is preferred that drying 12h under the conditions of 70 DEG C, moisture is not
7% must be crossed.According to《Chinese Pharmacopoeia》2015 editions the 4th (general rule 2302) is tested.The steamed sealwort processing procedure side of the present invention
The process of steamed sealwort is divided into multiple and different processing stages in method to handle, before this to the drying of sealwort pre-wash and
Advance drying and processing so that nutritional ingredient is containing in sealwort, then carries out five and steams five solarizations processing so that sealwort basically reaches steamed
Then sealwort, is dried to relatively low by the state of nutrients release and the sealwort maturation of processing when the 6th time steamed and drying
Moisture content level causes the quality of sealwort more preferably.In addition, steamed sealwort can be improved by controlling moisture in steamed sealwort
As the safe and effective time limit of health products storage, avoid storing improper caused rotten.
Preferably, sealwort total ash≤5% processed.Content of ashes control is steamed in clear soup in reduced levels, directly reaction
The quality grade of sealwort, processing procedure of the present invention fully clean sealwort, by the repeatedly steamed processing processing optimized and revised so that
Ash impurities content is extremely low in sealwort, the more outstanding protrusion of sealwort application effect.
Compared with prior art, beneficial effects of the present invention:
1. the present invention processes the method for steamed sealwort compared with existing sealwort processing procedure, pass through the steamed work of optimization design
Skill mode, realization prepare processing and steamed drying technique stage by stage in advance, it is more preferably excellent to process the sealwort quality being prepared
Show, either its mouthfeel eaten as health products or the content of the Natural Medicine Chemistry ingredient with health-care efficacy are all excellent
In sealwort decoction piece, stir-baked RHIZOMA POLYGONATI with yellow rice wine that existing process processes etc..
2. the present invention provides the method that sealwort is tested, with reference to quality heterosis after the steamed sealwort Preparation process of the present invention
Difference proposes that specific aim, which measures, processes steamed Siberian solomonseal rhizome polysaccharide, 5-HMF, diosgenin, extract, ash content and moisture equal size,
The content differences containing Natural Medicine Chemistry ingredient such as medicine materical crude slice, stir-baked RHIZOMA POLYGONATI with yellow rice wine are processed compared with existing sealwort with reference to steamed sealwort, it can
Whether the sealwort after being processed with better identification and analysis meets for the steamed sealwort concocting method processing gained of the present invention, it is ensured that steamed
The differentiation of sealwort and the sealwort of general processing procedure processing.
Description of the drawings:
Fig. 1 is glucose content standard curve.
Fig. 2 is that 5-HMF reference substance solution liquid chromatograms correspond to retention time.
Fig. 3 is sealwort sample liquid chromatogram, and wherein 5-HMF retention times are marked.
Fig. 4 is 5-HMF standard curves.
Fig. 5 is diosgenin reference substance standard curve.
Fig. 6 is diosgenin reference substance HPLC chromatogram, and wherein diosgenin retention time is marked.
Fig. 7 is sealwort sample liquid chromatogram, and wherein diosgenin retains peak separate marking.
Specific embodiment
Further, the steamed sealwort that the present invention is obtained for processing is detected using following 5-HMF assays mode
Analysis, determines the 5-HMF contents in the steamed sealwort cooked:
201:Reference substance solution is prepared, and precision weighs 5-HMF reference substances, and reference substance solution is made with methanol dissolving, is protected from light
Cord blood.
202:Test solution is prepared, and precision weighs sealwort, adds in 10mL methanol ultrasonic extraction 10-30min, is filtered, filter
Slag adds 10mL methanol ultrasonic extraction 10-30min, filtering.Merging filtrate is settled in 25mL measuring bottles.
203:Reference substance solution and test solution are tested using HPLC, 5-HMPF contents in sealwort are calculated.
Preferably, chromatographic condition is as follows:Yi Lite ODS-B chromatographic columns (250mm × 4.6mm, 5 μm);Mobile phase:Acetonitrile:
1% phosphoric acid water (5:95);Flow velocity:1.0ml/min;Detection wavelength:284nm;Column temperature:30℃;10 μ L of sample size.
For the test analysis wherein 5-HMF contents for sealwort of steaming in clear soup, determine whether steamed sealwort is fully processed, finished product
Whether quality, mouthfeel and health nutrient functional component are fully discharged, and realize the meaning for promoting product health-care efficacy.
Further, S3, Determination of Diosgenin in Rhizoma polygonati mensuration mode are as follows in detection process:
301:Reference substance solution is prepared, and precision weighs diosgenin reference substance, is prepared into reference substance with methanol dissolving, is kept away
Light Cord blood.
302:Test solution is prepared, and weighs Solomonseal Rhizome, is added in ethyl alcohol, is shaken up, weigh, be heated to reflux 2-5h, let cool,
It weighs, with ethyl alcohol deficiency weight, shakes up, filter.Filtrate is concentrated to dryness, and residue adds the dissolving with hydrochloric acid of 1-4mol/L, boiling water reflux
2-5h, cooling, moves in separatory funnel, adds in chloroform, extracts 2-5 time, and merging chloroformic solution is concentrated under reduced pressure into dry, residue adds
Enter methanol dissolving, be settled in 25mL volumetric flasks, shake up, obtain test solution.
303:Reference substance solution and test solution are tested using HPLC, Determination of Diosgenin in Rhizoma polygonati is calculated.
Preferably, chromatographic condition is as follows:Yi Lite ODS-B chromatographic columns (250mm × 4.6mm, 5 μm);Mobile phase:Acetonitrile:
Water=96:4;Flow velocity:1.0ml/min;Detection wavelength:203nm;Column temperature:30℃;Sample size is 10 μ L.
Diosgenin is the important foundation material composition of synthesizing steroid steroids, for enhancing anti-infective, antiallergy, resisting
The effect of virus and Hemorrhagic shock is of great significance, and health-care efficacy value is very big.It is processed and obtained using the detection of HPLC test methods
Steamed Determination of Diosgenin in Rhizoma polygonati, be conducive to promoted product quality grade, realize better healthcare applications potentiality.This
The HPLC test methods selected to be invented, are extracted by ethyl alcohol, acid is finally configured to methanol solution dissolved with solvent extraction processing,
Realize that accurate extraction Diosgenin in Rhizoma polygonati carries out the purpose of HPLC detection and analysis.It realizes for Chinese yam in steamed sealwort product
The accurate control of sapogenin content tests and analyzes and determines the true quality grade of diosgenin.
With reference to test example and specific embodiment, the present invention is described in further detail.But this should not be understood
Following embodiment is only limitted to for the scope of the above-mentioned theme of the present invention, it is all that this is belonged to based on the technology that present invention is realized
The scope of invention.
<Embodiment 1>
Steamed sealwort processes
(1) by fresh sealwort removal impurity and fibrous root, clean and dry for 24 hours, be placed in 40 DEG C of oven dryings for 24 hours, make its water
Point content reaches 25%, and sheet 6-8mm is cut in taking-up, then in 40 DEG C of baking ovens it is dry for 24 hours, its moisture is made to reach 19%.
(2) the dried sealwort of step 1 is cut into slices, is placed in and steams in container, steam 6h, taken out.65 DEG C of heated-air drying 16h are extremely
Moisture 17% steams one to get one and shines sealwort.
(3) repeat above step 2 and operate four times to get five steamings, five solarization sealworts.Sealwort water after second of steamed drying of control
Divide content 16%, third time 14%, the 4th time 12%, the 5th time 10%.
Five solarization sealworts of (4) five steaming, which are placed in, to be steamed in container, is steamed 6h, is taken out.75 DEG C of heated-air dryings for 24 hours, reach moisture
7% steams six to get six shines sealwort.
<Test 1>
Six, which steam six, shines 5-HMF assays in sealwort
201:Reference substance solution is prepared, and precision weighs 5-HMF reference substances, and reference substance solution is made with methanol dissolving, is protected from light
Cord blood.
202:Test solution is prepared, and precision weighs the sealwort of the processing of embodiment 1, adds in 10mL methanol ultrasonic extractions 10-
30min, filtering, filter residue add 10mL methanol ultrasonic extraction 10-30min, filter.Merging filtrate is settled in 25mL measuring bottles.
203:Reference substance solution and test solution are tested using HPLC.Chromatographic condition is as follows:Yi Lite ODS-B chromatographic columns
(250mm × 4.6mm, 5 μm);Mobile phase:Acetonitrile:1% phosphoric acid water (5:95);Flow velocity:1.0ml/min;Detection wavelength:284nm;
Column temperature:30℃;10 μ L of sample size.
It is 0.63mg/g that 5-HMF contents in sealwort, which are calculated,.
<Embodiment 2>
Steamed sealwort processes
(1) by fresh sealwort removal impurity and fibrous root, clean and dry 16h, be placed in 42 DEG C of oven drying 16h, make its water
Point content reaches 28%, and sheet 5-8mm is cut in taking-up, and then the dry 12h in 45 DEG C of baking ovens, makes its moisture reach 20%.
(2) the dried sealwort of step 1 is cut into slices, is placed in and steams in container, big fire steams 5h, takes out.70 DEG C of hot air dryings
Dry 12h steams one to get one and shines sealwort.
(3) above step 2 is repeated to operate twice.Then, sealwort is used instead slow boiling and is steamed using the identical operation of step 2;
It repeats slow boiling and steams drying 2 times, complete 5 steamed and drying operations in total, obtain five steamings five and shine sealwort.
Step 2-3 steams in clear soup in drying process sealwort moisture 18% after control steamed drying for the first time, second 17%,
15%, the 4th time 12%, the 5th time 10% for the third time.
Five solarization sealworts of (4) five steaming, which are placed in, to be steamed in container, and slow boiling steams 8h, takes out.78 DEG C of heated-air drying 22h, make moisture
Reach≤7% and steam six solarization sealworts to get six.
Six, which are steamed, using HPLC detection methods test six same as Example 1 shines sealwort, 5-HMF contents 0.62mg/g.
According to《Chinese Pharmacopoeia》2015 editions the 4th (general rule 2201) hot dippings are tested, and are measured by solvent of water, are surveyed
Test result shows water-soluble extractives content 54% in steamed sealwort, moisture 6.66%.
Glucose content in the steamed sealwort of test draws standard curve as shown in Figure 1, meter after dextrose standard sample test
Calculation obtains polyoses content 4.68%.
<Embodiment 3>
Steamed sealwort processes
(1) by fresh sealwort removal impurity and fibrous root, naturally dry 32h is cleaned, 36 DEG C of oven drying 30h is placed in, makes
Its moisture reaches 24%, and sheet 6-10mm is cut in taking-up, and then the dry 32h in 38 DEG C of baking ovens, reaches its moisture
17%-19%.
(2) the dried sealwort of step 1 is cut into slices, is placed in and steams in container, big fire steams 7h, takes out.62 DEG C of hot air dryings
Dry 14h steams one to get one and shines sealwort.
(3) above step 2 is repeated to operate twice.Then, sealwort is simply used instead slow boiling using the similar operation of step 2
Steam 8h, 70 DEG C of heated-air drying 10h;It repeats slow boiling and steams drying 2 times.5 steamed and drying operations are completed in total, obtain five steamings five
Shine sealwort.
Step 2-3 steams in clear soup in drying process sealwort moisture 18% after control steamed drying for the first time, second 17%,
15%, the 4th time 13%, the 5th time 11% for the third time.
Five solarization sealworts of (4) five steaming, which are placed in, to be steamed in container, and slow boiling steams 8h, takes out.58 DEG C of heated-air drying 30h, make moisture
Reach≤7% and steam six solarization sealworts to get six.
It detects obtained six and steams six solarization sealworts, 5-HMF contents 0.65mg/g.
<Test 2>
Determination of Diosgenin measures
Diosgenin is steroid sapogenin, and steroid sapogenin indissoluble or not soluble in water is soluble in methanol, ethyl alcohol, chloroform
Wait organic solvents.
1. the preparation of reference substance solution
Take diosgenin reference substance appropriate, accurately weighed, the reference substance being prepared into methanol dissolving;0.844mg/ml is molten
Liquid.It is protected from light Cord blood.
2. the preparation of test solution
The sealwort that Example 3 processes, milling, precision weigh powder about 2g, put and add 50mL ethyl alcohol in boiling flask, shake
It is even, it weighs, is heated to reflux 4h, let cool, weigh, supply weight with ethyl alcohol, shake up, filter.Filtrate 20mL is concentrated to dryness, residue
Add 80mL, the dissolving with hydrochloric acid of 3mol/L, boiling water reflux 4h is cooled down, moved in separatory funnel, chlorination imitates 40mL (20,10,10mL)
Extraction 3 times merges chloroform solution, and be concentrated under reduced pressure dry chloroform, and residue adds methanol to dissolve, and is settled in 25mL volumetric flasks, shakes up, with height
Effect liquid phase chromatogram method measures.
3. chromatographic condition
Yi Lite ODS-B chromatographic columns (250mm × 4.6mm, 5 μm);Mobile phase:Acetonitrile:Water (96:4);Flow velocity:1.0ml/
min;Detection wavelength:203nm;Column temperature:30℃;Sample size is 10 μ l.
4. linear relationship is investigated
Precision draws 2,4,6,8,10, the 12 μ L of diosgenin reference substance solution of above-mentioned preparation, injects liquid chromatograph
In, diosgenin retention time is determined, wherein the liquid chromatogram of 2 μ L sample sizes is as shown in Figure 6.Then, it is different right to measure
Chromatographic peak area is measured according to product solution injection rate, is that ordinate draws standard curve using sample size as abscissa, peak area, as a result
As shown in figure 5, be fitted equation of linear regression is:Y=336438x+53652 (R=0.9991), the results showed that, Dioscin
Member is good with peak area linear relationship in 1.69-10.13 μ g ranges.
5. experimental result
It weighs above-mentioned test solution and analysis, wherein sealwort liquid phase is detected under reference substance solution identical chromatographic conditions
Chromatogram is as shown in Figure 7.According to liquid chromatogram measuring diosgenin peak area, calculate and determine Chinese yam in each steamed sealwort sample
Sapogenin content, the results are shown in table below.
Table 4 is steamed in clear soup Determination of Diosgenin in Rhizoma polygonati
Steamed Determination of Diosgenin in Rhizoma polygonati is tested and analyzed using HPLC chromatogram method, Determination of Diosgenin 1.63%,
Water-soluble extractives content 53.01%, moisture 6.72%.
<Embodiment 4>
Steamed sealwort processes
(1) fresh sealwort is removed into impurity and fibrous root, cleans and dry 12h, be placed in 40 DEG C of baking ovens, dry 26h makes its water
Point content reaches 27%, and sheet 6-9mm is cut in taking-up, and then the dry 18h in 40 DEG C of baking ovens, makes its moisture reach 22%.
(2) the dried sealwort of step 1 is cut into slices, is placed in and steams in container, steam 5h, taken out.60 DEG C of heated-air dryings, it is dry
12h makes its moisture reach 18% and steams a solarization sealwort to get one.
(3) repeat above step 2 and operate four times to get five steamings, five solarization sealworts.
In step 2-3, after steaming sealwort each time, the dry degree for making the reduction of its moisture gradually rises, for the first time
Dry moisture 18% is steamed, second 17%, third time 15%, the 4th time 12%, the 5th time 10%.It is steamed by five times
And after drying process, moisture continuously decreases in sealwort, and sealwort, which processes degree, gradually to be deepened, more in the sealwort processed of steaming in clear soup
Sugared content reduces, and sealwort mouthfeel speed improves, and the 5-HMF contents for representing processing quality quickly improve.
Five solarization sealworts of (4) five steaming, which are placed in, to be steamed in container, is steamed 4-8h, is taken out.70-80 DEG C of heated-air drying, makes moisture
Reach 7% and steam six solarization sealworts to get six.
Obtained six, which steam six, shines in sealwort, Determination of Diosgenin >=1.5%, polyoses content 4.72%, moisture
6.58%, total ash content 3.94%.
<Test 3>
Steamed sealwort detection method:5-HMF assays
(5-HydroxyMethylFurfural, 5-HMF are a kind of thermal degradation products of sugar to 5 hydroxymethyl furfural, containing sugar
Chinese medicine preparation during be likely to generate, it is closely related with concocted time and temperature, be that one kind may be used to indicate processing journey
The substance of degree, as the active ingredient of Chinese medicine preparation principle research.
1. the preparation of reference substance solution
Take 5-HMF reference substances appropriate, accurately weighed, the 20.96 μ g/mL of 5-HMF reference substances being prepared into methanol dissolving are molten
Liquid is protected from light Cord blood.
2. the preparation of test solution
Precision weighs the sealwort of the preparation of Example 4, and about 0.2g is put in 150m conical flask with cover, and precision adds in methanol
10mL, ultrasonic extraction 20min, filtration.Filter residue adds methanol 10mL, ultrasonic extraction 10min, and filtration, filtrate is settled to 25mL measuring bottles
In to get.
3. chromatographic condition
Yi Lite ODS-B chromatographic columns (250mm × 4.6mm, 5 μm);Mobile phase:Acetonitrile:1% phosphoric acid water (5:95);Flow velocity:
1.0ml/min;Detection wavelength:284;Column temperature:30℃;Sample size is 10 μ L.
4. linear relationship is investigated
Precision weighs 5 hydroxymethyl furfural reference substance, and the 5 hydroxymethyl furfural that concentration is 20.96 μ g/ml is configured to methanol
Reference substance solution.It is detected using HPLC liquid chromatograies, measure obtains 5-HMF retention times, and the results are shown in Figure 2.Then,
Precision draw 2,4,6,8,10,12 μ L of this liquid, inject liquid chromatograph in, measure chromatographic peak area, using sample size as abscissa,
Peak area draws standard curve for ordinate, and the results are shown in Figure 4, obtains equation of linear regression and is:Y=187675x-9603.1
(R2=0.9999), as a result surface, 5-HMF are good with peak area linear relationship in 0.04-0.25 μ g ranges.
5. experimental result
Steamed sealwort test sample is detected analysis with HPLC, survey wherein sealwort liquid chromatogram as shown in figure 3, according to
The 5-HMF that HPLC is measured retains peak area, brings above-mentioned equation of linear regression into, 5-HMF contents in steamed sealwort are calculated, and ties
Fruit is as shown in the table.
Table 3 is steamed in clear soup 5-HMF contents in sealwort
<Comparative example 1>
Natural sealwort
Fresh natural sealwort is taken, peace and quiet, naturally dry 48h is used《Chinese Pharmacopoeia》2015 editions the 4th general rules,
HPLC, ultra-violet and visible spectrophotometer test and analyze fresh Diosgenin in Rhizoma polygonati, 5-HMF, water-soluble extractives and contain
Amount, polyoses content, moisture, content of ashes, it is as a result as follows:
Fresh natural sealwort, which is cleaned, dries sample test, diosgenin 0.052%, 5-HMF 0%, water-soluble extractives
Content 42%, polyoses content 11.65%, moisture 38%, content of ashes 4.8%.
<Comparative example 2>
Traditional handicraft steams sealwort
Fresh natural sealwort is taken, peace and quiet, for 24 hours, steam in clear soup naturally dry 8h, steams completion and dries 2h later, then 45 DEG C
Heated-air drying 8h is prepared a steaming one and shines sealwort.
Using《Chinese Pharmacopoeia》2015 editions the 4th general rule, HPLC, ultra-violet and visible spectrophotometers, detection and analysis are fresh
Diosgenin in Rhizoma polygonati, 5-HMF, the content of water-soluble extractives, polyoses content, moisture, content of ashes, as a result such as
Under:
Sealwort sample test, diosgenin 0.048%, 5-HMF 0.02%, the content 46%, more of water-soluble extractives
Sugared content 8.26%, moisture 13%, content of ashes 4.3%.
<Comparative example 3>
Nine, which steam nine, shines sealwort
Fresh natural sealwort is taken, peace and quiet, naturally dry for 24 hours, is steamed in clear soup 6h with water, steams completion and be placed on hot air drier
In 45 DEG C of heated-air drying 4h, realize one steam one shine.Steamed, drying process 8 times is repeated, nine steamings nine are prepared and shine sealwort.This is right
During ratio steams sealwort and the Main Differences of embodiment are after in steamed and drying process not to drying each time
Sealwort moisture is controlled.
Using《Chinese Pharmacopoeia》2015 editions the 4th general rule, HPLC, ultra-violet and visible spectrophotometers, detection and analysis are fresh
Diosgenin in Rhizoma polygonati, 5-HMF, the content of water-soluble extractives, polyoses content, moisture, content of ashes, as a result such as
Under:
Sealwort sample test, diosgenin 0.055%, 5-HMF 0.08%, the content 48%, more of water-soluble extractives
Sugared content 3.75%, moisture 8%, content of ashes 3.8%.
<Comparative example 4>
Process stir-baked RHIZOMA POLYGONATI with yellow rice wine
Fresh natural sealwort is taken, peace and quiet, naturally dry carries out steaming 6h for 24 hours, with yellow rice wine, steams completion and dries 2h later,
Then 45 DEG C of heated-air drying 8h, are prepared stir-baked RHIZOMA POLYGONATI with yellow rice wine.
Using《Chinese Pharmacopoeia》2015 editions the 4th general rule, HPLC, ultra-violet and visible spectrophotometers, detection and analysis are fresh
Diosgenin in Rhizoma polygonati, 5-HMF, the content of water-soluble extractives, polyoses content, moisture, content of ashes, as a result such as
Under:
Sealwort sample test, diosgenin 0.052%, 5-HMF 0.04%, the content 51%, more of water-soluble extractives
Sugared content 7.68%, moisture 11%, content of ashes 4.1%.
The sealwort prepared by comparing a variety of different sealwort concocting methods, the polysaccharide drawn with reference to detection and analysis test,
5-HMF, the content of diosgenin and extract, moisture, grey gradation parameter.The present invention processes sealwort technique, is steamed using six
The mode of six solarization optimizing technology parameters is processed, and polyoses content is compared with the sealwort not processed, and polyoses content reduces, through undue
The content of Siberian solomonseal rhizome polysaccharide after high-quality sealwort processes is analysed, it is specified that polyoses content is not less than 4% after processing;There is 5-HMF anti-cardiac muscle to lack
Blood, anti-oxidant, hypoglycemic, change hemorheological property and neuroprotective, have certain effect to human body, therefore can be used as big gun
For one standard of processing procedure degree, it is necessary to be measured to its content, the content of high-quality sealwort must not be less than 0.50mg/g;Dioscin
First steroid saponin constituents include the sapogenins such as diosgenin, sarsasapogenin, mainly based on diosgenin, after processing
Compared with the sealwort not processed, content reduces the Determination of Diosgenin of sealwort, the Dioscin after sealwort processes by analysis
First content, Determination of Diosgenin must not be less than 1.5mg/g after now providing high-quality processing;Extract must not be less than 50%, moisture
7% must not be higher than, ash content must not be higher than 5%.
Claims (10)
1. a kind of steamed sealwort concocting method, comprises the following steps:
(1)By fresh sealwort removal impurity and fibrous root, clean and dry 12-36h, be placed in 30-50 DEG C of baking oven, dry 12-
36h makes its moisture reach 25-40%;
Sheet 5-10mm is cut in taking-up, and then the dry 12-36h in 40 DEG C of baking ovens, makes its moisture reach 15-24%;
(2)The dried sealwort of step 1 is cut into slices, is placed in and steams in container, steams 4-8h, is taken out;
55-80 DEG C of heated-air drying, dry 10-20h make its moisture reach 12-15% and steam a solarization sealwort to get one;
(3)It repeats above step 2 and operates four times to get five steamings, five solarization sealworts;
(4)Five steamings, five solarization sealworts, which are placed in, to be steamed in container, is steamed 4-8h, is taken out;70-80 DEG C of heated-air drying, reaches moisture
7% steams six to get six shines sealwort;
Obtained six, which steam six, shines in sealwort, 5-HMF contents >=0.6mg/g.
2. steamed sealwort concocting method as described in claim 1, which is characterized in that step 1, clean and dry 20-26h, be placed in 38-
In 45 DEG C of baking ovens, dry 15-26h makes its moisture reach 25-35%.
3. steamed sealwort concocting method as described in claim 1, which is characterized in that step 1, take out by dry sealwort, cut
7-9mm sheets, then the dry 12-30h in 35-45 DEG C of baking oven, makes its moisture reach 17-24%.
4. steamed sealwort concocting method as described in claim 1, which is characterized in that step 1, sealwort slice thickness 5-9mm.
5. steamed sealwort concocting method as claimed in claim 4, which is characterized in that slice thickness 6-8mm.
6. steamed sealwort concocting method as described in claim 1, which is characterized in that during sealwort steams, 3 times steam use
Big fire is steamed in clear soup, and rear 3 uses slow boiling is steamed in clear soup, and is steamed in total 6 times.
7. steamed sealwort concocting method as described in claim 1, which is characterized in that step 2, the section of dried sealwort is placed in steaming
In container, 5-7h is steamed, then 57-65 DEG C of heated-air drying, dry 12-18h makes its moisture reach 12-15% to get one
It steams one and shines sealwort.
8. steamed sealwort concocting method as described in claim 1, which is characterized in that step 4, in the sealwort processed, Chinese yam
Sapogenin content >=1.5%.
9. steamed sealwort concocting method as described in claim 1, which is characterized in that step 4, the sealwort processed is water-soluble
Extract content >=50%.
10. steamed sealwort concocting method as described in claim 1, which is characterized in that step 4, the sealwort moisture processed contains
Amount≤7%.
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