CN107296891A - Stir-baked RHIZOMA POLYGONATI with yellow rice wine integration Habitat producing and concocting method - Google Patents
Stir-baked RHIZOMA POLYGONATI with yellow rice wine integration Habitat producing and concocting method Download PDFInfo
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Abstract
The present invention relates to the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine and concocting method, the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；Clean cadmium yellow essence is put in boiling water and scalded 3 10 minutes, sheet is then directly cut into, airing is half-dried；Yellow rice wine, vexed profit 15 hours are sprayed on the sealwort sheet cut again；Then the vexed sealwort moistened is placed in again and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 hours " steamed vexed dry in the air " 29 times repeatedly, gets product stir-baked RHIZOMA POLYGONATI with yellow rice wine.The technique of invention is by Habitat producing and stir-baked RHIZOMA POLYGONATI with yellow rice wine technique, the stir-baked RHIZOMA POLYGONATI with yellow rice wine steady quality of production is homogeneous, the production cycle can effectively be shortened, reduce energy resource consumption and human cost, continuous production can be achieved, and preferably can be applied in industrialized production, while the stir-baked RHIZOMA POLYGONATI with yellow rice wine antioxidation activity processed according to the inventive method is significantly better than commercially available stir-baked RHIZOMA POLYGONATI with yellow rice wine.
Description
Technical field
The invention belongs to Chinese medicine processing, process field, more particularly to the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine and concocting method.
Background technology
, it is necessary to be processed into medicine materical crude slice according to actual needs after sealwort harvesting, preservation, transport, packing and clinic could be facilitated
Use；Traditional sealwort decoction piece processing method is usually cutting and drying, but in process, it is not easily-controllable with oven for drying
Drying degree processed, easily causes active ingredient loss.Patent document (CN104623274A) discloses the processing of sealwort Habitat producing
Integrated new technology, fibrous root is cut off by sealwort medicinal material, clean be dried to after the impurity such as silt with solar energy at 40-60 DEG C 6-7 into
It is dry, then sealwort is cut into 4-8mm sheet, then dried with solar energy at 40-60 DEG C, finally packed.So can be with
The problem of solving traditional processing technology cannon system, it is difficult to control temperature, and need to consume the substantial amounts of energy.But, wine
Sealwort is clinically using more, to stir-baked RHIZOMA POLYGONATI with yellow rice wine more careful description in 2008 Nian Ban Beijing prepared slices of Chinese crude drugs concocted specifications：Take
Crude drug, removes impurity, and size is separated, plus yellow rice wine is mixed thoroughly, vexed profit 4-8 hours, loads in steaming pot, sealing, water proof heating or use
Steam is heated, and is steamed 24~32 hours, is sucked to yellow rice wine, during the black profit of color and luster, is taken out, is slightly dried in the air, cut sheet, is dried.It is net per 100kg
Sealwort, uses yellow rice wine 20kg.But there is no researcher to enter sealwort medicinal material Habitat producing with being processed into the technique of stir-baked RHIZOMA POLYGONATI with yellow rice wine at present
Row Study on Integration, to save production routine, shortens the production cycle, saves human and material resources, and then improve production efficiency.
The content of the invention
The purpose of the present invention is to overcome the weak point and defect of existing stir-baked RHIZOMA POLYGONATI with yellow rice wine Habitat producing technology there is provided a kind of technique
Simply, the integrated Habitat producing of quality controllable stir-baked RHIZOMA POLYGONATI with yellow rice wine and concocting method.
The technical scheme that the present invention takes is：Stir-baked RHIZOMA POLYGONATI with yellow rice wine integration Habitat producing and concocting method, comprise the following steps：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 3-10 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine, vexed profit 1-5 hours are sprayed on the sealwort sheet cut again；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 2-9 times repeatedly, produce.
It is preferred that, it is 5 minutes that step (2) the sealwort sheet, which puts in boiling water the ironed time,.
It is preferred that, step (3) the yellow rice wine consumption is the 20% of sealwort weight, and the vexed profit time is 2 hours.
It is preferred that, step (4) " steaming-vexed-dry in the air " number of times is 2 times.
Further preferably, the integrated Habitat producing of described stir-baked RHIZOMA POLYGONATI with yellow rice wine and concocting method, it is characterised in that including following step
Suddenly：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 5 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine is sprayed on the sealwort sheet cut again, vexed profit 2 hours, wherein yellow rice wine consumption are sealwort weight
20%；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 2 times repeatedly, produce.
The present invention also provides a kind of TLC Identification of stir-baked RHIZOMA POLYGONATI with yellow rice wine, it is characterised in that：
The preparation of reference substance solution：Diosgenin reference substance is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol dissolving
And scale is settled to, shake up, concentration is made for 0.2mgmL-1Solution, produce；
The preparation of need testing solution：By sample comminution, 24 mesh sieves are crossed, test sample medicinal powder is obtained.Test sample medicinal powder 5.0g is weighed,
Put in flask, plus ethanol 50mL refluxing extraction 1h, suction filtration, filtrate adds hydrochloric acid 5mL to be heated to reflux 2h, after cooling, uses 40% hydrogen-oxygen
It is 7.0 to change sodium solution to be adjusted to pH, and water bath method solvent, residue heating water 40mL makes dissolving, and chlorination imitates extraction 3 times repeatedly, every time
30mL, combining extraction liquid, water-bath volatilizes chloroform, and residue adds methanol 10mL to make dissolving, shaken up, produces.
According to thin-layered chromatography experiment, draw reference substance solution and each 5 μ l of need testing solution are put in same silica G thin layer respectively
On plate, with cyclohexane-ethyl acetate-formic acid (4:1:0.1) mixed solution be development system, deploy, take out, dry, spray with
10% phosphomolybdic acid ethanol solution is developed the color, and clear spot is heated in 105 DEG C.
The advantage and beneficial effect of the present invention：
The technique of invention is by Habitat producing and stir-baked RHIZOMA POLYGONATI with yellow rice wine technique, and the stir-baked RHIZOMA POLYGONATI with yellow rice wine steady quality of production is homogeneous, can effectively contract
Short production cycle, reduction energy resource consumption and human cost, can be achieved continuous production, and it is big raw to be preferably applied to industrialization
In production, while the stir-baked RHIZOMA POLYGONATI with yellow rice wine antioxidation activity processed according to the inventive method is significantly better than commercially available stir-baked RHIZOMA POLYGONATI with yellow rice wine.
First, quality standard research
This research using 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice as research object,《Chinese Pharmacopoeia》On the basis of versions in 2015, wine is improved
Sealwort decoction piece quality standard, the reasonability for evaluation stir-baked RHIZOMA POLYGONATI with yellow rice wine process of preparing technique provides foundation.
1. materials and methods
1.1 material
1.1.1 laboratory apparatus
The type balance of AT2 family expenses 10 (Hua Ying weighing apparatus Co., Ltd), (Guangdong is beautiful for beautiful HT2115HM types multifunctional electromagnetic oven
Living electric apparatus Manufacturing Co., Ltd), (Zhejiang Ai Shida electrical equipment shares are limited for two layers of multiple bottom steamer of Ai Shida NK1528 types stainless steel
Company), XFB-200 Universalpulverizers (Hunan Zhong Cheng pharmaceutical machines factory), Ao Haosi AR1140 type electronic balance (precision：Ten thousand
/ mono-, Mettler-Toledo Instrument (Shanghai) Co., Ltd.), GZX-9140MBE types electric drying oven with forced convection (Beijing Hai Tian
You Cheng Science and Technology Ltd.s), the box Muffle furnaces of SG-XS (Shanghai Shi Jie electric furnaces Co., Ltd), HH-2 type electric-heated thermostatic water baths
(Ke Wei Yongxings, Beijing Instrument Ltd.), UV-2600 ultraviolet-visible spectrophotometers (SHIMADZU companies), S500T-
The mesh biomicroscope of 530HS types three (Suzhou Bei Tejia Electro-optical Technology, INC. (US) 62 Martin Road, Concord, Massachusetts 017)
1.1.2 test reagent reagent
Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice (commercially available, to be purchased from Xi'an, the major pharmacies in Xianyang), the raw sealwort medicinal material (place of production：Shaanxi, is purchased from Xi'an
City's ten thousand longevity road medicinal material market), shao-hsing rice wine (commercially available, to be purchased from everybody happy supermarket of Xianyang), DEXTROSE ANHYDROUS reference substance (purity >=
99%, lot number：S08J6G1), diosgenin reference substance (purity >=98%, lot number：P20J7F18116) (given birth to by Chinese medicine
Tetramune research institute provides), methanol, ethanol, absolute ethyl alcohol, n-butanol, hexamethylene, ethyl acetate, formic acid, hydrochloric acid, sulfuric acid, height
Chloric acid, anthrone, phosphomolybdic acid, silver nitrate (being that analysis is pure), purified water (Xianyang Dong Sheng drinks Co., Ltd), sealwort medicinal material is through Shan
It is yellow that western Chinese traditional medicine identification teaching and research room of pharmaceutical college of university of TCM professor Hu Benxiang is accredited as Liliaceae Polygonatum herbaceos perennial
Smart Polygonatum sibiricum Red. rhizome, practises and claims " polygonatum sibiricum Redoute ".
1.1.3 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice information (table 1)
The stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice information table of table 1
1.2 method
1.2.1 stir-baked RHIZOMA POLYGONATI with yellow rice wine character
10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice are observed, its feature substantially conforms to pharmacopeia description.
1.2.2 stir-baked RHIZOMA POLYGONATI with yellow rice wine differentiates
(1) microscopical characters
Using《Chinese Pharmacopoeia》10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice are carried out by the microscopical characters method of four ruless of preparations of version in 2015 2001
Powder differentiates.
(2) thin layer differentiates
The preparation of reference substance solution：Take diosgenin reference substance appropriate, it is accurately weighed, put in 10mL measuring bottles, plus methanol
Dissolve and be settled to scale, shake up, concentration is made for 0.2mgmL-1Solution, produce.
Distilled spirits sealwort decoction piece：Take sealwort medicinal material appropriate, wash quickly is net, plus (amount of taking is medicinal material amount to shao-hsing rice wine
20%) mix thoroughly, put in Stainless steel basin and be capped after vexed 30min, put in steamer, steam after 48h, then vexed 12h, to the black profit of color and luster, it is cut into 2
~4mm sheet, puts in baking oven and is dried under the conditions of 60 DEG C, takes out, produces.
The preparation of need testing solution：By sample comminution, 24 mesh sieves are crossed, test sample medicinal powder is obtained.Test sample medicinal powder 5.0g is weighed,
Put in flask, plus ethanol 50mL refluxing extraction 1h, suction filtration, filtrate adds hydrochloric acid 5mL to be heated to reflux 2h, after cooling, uses 40% hydrogen-oxygen
It is 7.0 to change sodium solution to be adjusted to PH, and water bath method solvent, residue heating water 40mL makes dissolving, and chlorination imitates extraction 3 times repeatedly, every time
30mL, combining extraction liquid, water-bath volatilizes chloroform, and residue adds methanol 10mL to make dissolving, shaken up, produces.
According to thin-layered chromatography experiment, draw reference substance solution and each 5 μ l of need testing solution are put in same silica G thin layer respectively
On plate, with cyclohexane-ethyl acetate-formic acid (4:1:0.1) mixed solution be development system, deploy, take out, dry, spray with
10% phosphomolybdic acid ethanol solution is developed the color, and clear spot is heated in 105 DEG C.
Thin layer discriminating is carried out to 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice respectively, this method is verified according to its chromatographic behavior on lamellae
Feasibility.
Using different batches stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice, the feasibility of this method is investigated according to 1.2.2.2 lower methods：
The tolerance of lamellae is investigated：Qingdao Haiyang chemical industry subsidiary factory (lot number is respectively adopted：20160402) with Qingdao wave
Silica-gel desiccant Co., Ltd (lot number：20150601) silica gel g thin-layer plate of production, this method is investigated by contrasting chromatographic behavior
Lamellae tolerance.
The tolerance of temperature is investigated：The chromatographic behavior of observation contrast this method respectively under the conditions of 40 DEG C and 4 DEG C, investigates this
The temperature tolerance of method.
The tolerance of humidity is investigated：The chromatographic behavior of observation contrast this method respectively under the conditions of 72%, 50%, 18%,
Investigate the humidity tolerance of this method.
1.2.3 determination of extractives
Using《Chinese Pharmacopoeia》The four lower hot dippings of the Extract mensurations of rules of preparations 2201 of version in 2015, successively with
Water, Diluted Alcohol, n-butanol are that solvent determines 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice extracts, analyze experimental result and determine water solubility respectively
Extract, Diluted Alcohol extract and n-butanol extract content limit (every batch of sample does 2 parts of Duplicate Samples).
1.2.4 ash determination
Using《Chinese Pharmacopoeia》Four Ash determination methods of rules of preparations 2302 of version in 2015, determine 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine drinks respectively
Piece total ash and acid-insoluble ash, analyze experimental result and determine total ash, acid-insoluble ash content limit (per lot sample
Product do 3 parts of Duplicate Samples).
1.2.5 determination of moisture
Using《Chinese Pharmacopoeia》Four aquametries of rules of preparations 0832 (the second method) of version in 2015, determine 10 batches respectively
Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice moisture, analyzes experimental result and determines moisture limit (every batch of sample does 3 parts of Duplicate Samples).
1.2.6 assay
(1) total starches assay
The preparation of reference substance solution learns from else's experience 105 DEG C of dryings to the DEXTROSE ANHYDROUS reference substance 33mg of constant weight, accurately weighed, puts
In 100mL measuring bottles, it is dissolved in water and is diluted to scale, shake up, produces and (contain DEXTROSE ANHYDROUS 0.33mg in per lmL).
The measure precision of standard curve measures reference substance solution 0.1mL, 0.2mL, 0.3mL, 0.4mL, 0.5mL, 0.6mL,
Put respectively in 10mL tool plug scale test tubes, respectively add water to 2.0mL, shake up, 0.2% Anthrone Sulphuric acid is slowly added dropwise in ice-water bath
Solution is mixed to scale, is let cool in rearmounted water-bath and is incubated 10 minutes, is taken out, and is put in ice-water bath and is cooled down 10 minutes immediately, is taken out,
Using corresponding reagent as blank.According to UV-VIS spectrophotometry (general rule 0401), absorbance is determined at 582nm wavelength.To inhale
Luminosity is ordinate, and concentration is abscissa, draws standard curve.
The preparation of need testing solution takes 60 DEG C of dryings to this product fine powder about 0.25g of constant weight, accurately weighed, puts round-bottomed flask
In, plus 80% ethanol 150mL puts and is heated to reflux in water-bath 1 hour, filtered while hot, and residue washs 3 times with 80% hot ethanol, often
Secondary 10mL, floods residual and filter paper is put in flask, add water 150mL, puts and is heated to reflux in boiling water bath 1 hour, is filtered while hot, residue and
Flask hot wash 4 times, each 10mL, merging filtrate and washing lotion, let cool, are transferred in 250mL measuring bottles, add water to scale,
Shake up, produce.
Assay precision measures need testing solution 1mL, puts 10mL tool plugs and dries in test tube, the preparation of sighting target directrix curve
Under method, from " adding water to 2.0mL ", absorbance being determined in accordance with the law, containing anhydrous from need testing solution is read on standard curve
The weight (mg) of glucose, calculates, produces.Analysis experimental result simultaneously determines polyoses content limit.
(2) total saponin content is determined
The preparation of reference substance solution：Take diosgenin reference substance appropriate, it is accurately weighed, it is placed in 5mL volumetric flasks, plus first
Alcohol dissolves and is settled to scale, shakes up, and produces concentration for 0.208mgmL-1Diosgenin standard items mother liquor, then add methanol dilute
Concentration is interpreted into for 0.104mgmL-1Reference substance solution.
The measure precision of standard curve measure reference substance solution 0.10mL, 0.10mL, 0.20mL, 0.25mL, 0.30mL,
0.30mL, 0.40mL, put in the test tube of dried and clean respectively, and water-bath volatilizes methanol, add perchloric acid 5.0mL, mix, in 25 DEG C
React 25 minutes, take out, using corresponding reagent as blank in water-bath.According to UV-VIS spectrophotometry (general rule 0401),
Absorbance is determined at 409nm wavelength.Standard curve is drawn in accordance with the law.
The preparation of need testing solution：Medicinal powder 1g is weighed, is placed in tool 50mL beakers, plus 80% ethanol 30mL, preservative film envelope
Mouthful, in 60 DEG C of ultrasonic extraction 3h, suction filtration, filtrate is transferred in 50mL volumetric flasks and is settled to scale, shake up, produces.
Assay precision measures need testing solution 0.5mL, puts in dried and clean test tube, under the preparation of sighting target directrix curve
Method, from " perchloric acid 5.0mL " is added to rise, according to UV-VIS spectrophotometry (general rule 0401), the survey at 409nm wavelength
Determine absorbance.The weight (m g) containing total saposins from need testing solution is read on standard curve, calculates, produces.Analysis experiment knot
Fruit simultaneously determines total saponin content limit.
2. result
The character of 2.1 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
Stir-baked RHIZOMA POLYGONATI with yellow rice wine finished product sheet type is in irregular sheet.Surface sepia, accidental gloss, tendon and vessel dot is high-visible.Touch
Softness.Mouth gustation sweet tea, that smells has the faint scent of wine, with《Chinese Pharmacopoeia》(version in 2015) stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice recorded
Character is basically identical.
The discriminating of 2.2 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
2.2.1 micro-powder differentiates
Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice micro-powder differentiates visible needle-like calcium oxalate crystal beam.
2.2.2 thin layer differentiates
(1) sample indentification by TLC result
According to the experimental method determined under " 1.2.2 (2) " item, using diosgenin as reference substance, 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine are drunk
Piece carries out indentification by TLC.As a result show, chromatographic behavior and the diosgenin reference substance of 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice samples
Chromatographic behavior is consistent, and each spot can preferably realize separation.
(2) tolerance is investigated
The investigation of lamellae is yellow with diosgenin reference substance and wine according to the experimental method determined under " 1.2.2 (2) " item
Smart medicine materical crude slice 3,4, No. 7 samples are investigated to lamellae tolerance.From investigation result, reference substance and sample are in separate sources
Lamellae on chromatographic behavior it is basically identical, each spot separating degree is preferable.
The experimental method that the investigation of temperature is determined according to 1.2.2.2, with diosgenin reference substance and stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice 3,
4th, No. 7 samples are investigated to temperature tolerance.From investigation result, reference substance and the sample color under high temperature and low temperature environment
Spectrum behavior is basically identical, and each spot separating degree preferably, has preferable adaptability under illustrating this law in high temperature and low temperature environment.
The experimental method that the investigation of humidity is determined according to " 1.2.2 (2) ", with diosgenin reference substance and stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
3rd, 4, No. 7 samples are investigated to humidity tolerance.From investigation result, reference substance and sample high humidity, in wet, low humidity ring
Chromatographic behavior is basically identical under border, and each spot separating degree preferably, illustrates that this law has preferable adaptability under different humidity environment.
2.3 determination of extractives
According to the 1.2.3 lower experimental methods determined, assay is carried out to the extract of 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice, in reality
Test on the basis of result and carry out statistical analysis, as a result such as table 2：
The determination of extractives result of table 2
2.4 ash determination
According to the 1.2.4 lower experimental methods determined, total ash, acid-insoluble ash content to 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
It is measured, statistical analysis is carried out on the basis of experimental result, as a result such as table 3：
The ash measured result of table 3
2.5 determination of moisture
According to the 1.2.5 lower experimental methods determined, the moisture to 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice is measured, in experiment
As a result statistical analysis is carried out on the basis of, as a result such as table 4：
The determination of moisture result of table 4
2.6 assay
According to the 1.2.6.1 and 1.2.6.2 lower experimental method determined, the extract of 10 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice is carried out respectively
Assay, carries out statistical analysis on the basis of experimental result.
2.6.1 total starches assay
Total starches determine gained regression equation：Y=4.8346X+0.0223, r=0.9993, as a result show that glucose exists
Linear relationship is good in the range of 0.33~1.98mg/mL.Each sample total starches measurement result such as table 5.
The total starches assay result of table 5
2.6.2 total saponin content is determined
Total saposins determine gained regression equation：Y=2.3786X-0.0522, r=0.9990, as a result show that total saposins exist
Linear relationship is good in the range of 0.104~0.416mg/mL.Each sample total saposins measurement result such as table 6：
The total saponin content measurement result of table 6
3. discuss
(1) the TLC discrimination methods of using in sealwort characteristic chemical constituent diosgenin as control, the method specificity are added
By force, adaptability is good.
(2) Diluted Alcohol extract is determined in accordance with the law, as a result meets its requirement, water-soluble extractives, n-butanol are added with method
The assay of extract.
(3) total ash is determined in accordance with the law, and measurement result has been done corresponding adjustment with reference to actual on the basis of standards of pharmacopoeia, increased
The content limit inspection of acid-insoluble ash.
(4) the method determination sample water content of general rule 0,832 second is used, as a result meets States Pharmacopoeia specifications.
(5) polyoses content is determined in accordance with the law, and corresponding adjustment has as a result been done on the basis of standards of pharmacopoeia with reference to actual, meanwhile, look into
Document discovery is read, is added in recent years for saponin component in sealwort containing having been reported that quantifier elimination to total saponin content more
Determine.
4. conclusion
This research, which has been augmented by reference substance TLC of diosgenin, to be differentiated, experimental method have passed through tolerance investigation, checking
The method is accurate, reliably, strong adaptability.
Diluted Alcohol determination of extractives result is 61.85%~81.15%, is met《Chinese Pharmacopoeia》Wine as defined in versions in 2015
Sealwort decoction piece ethanol soluble extractives must not be less than 45.0% requirement.Water-soluble extractives measurement result be 67.32%~
80.00%, in view of《Chinese Pharmacopoeia》Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice water-soluble extractives content is not specified, this quality standard is fixed tentatively water-soluble
Property extract must not be less than 55.0%.N-butanol determination of extractives result is 16.26%~43.03%, in view of《Chinese Pharmacopoeia》
Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice n-butanol extract content is not specified, this quality standard is fixed tentatively n-butanol extract and must not be less than
10.0%.
Total ash measurement result is 1.64%~5.19%,《Chinese Pharmacopoeia》Total ash in version proof spirit medicine materical crude slice in 2015
4.0% must not be crossed, with reference to this result of study, 5.5% must not be crossed for total ash by fixing tentatively.Acid-insoluble ash measurement result is
0.30%~1.43%, in view of《Chinese Pharmacopoeia》Acid-insoluble ash limitation is not specified, this quality standard fixes tentatively stir-baked RHIZOMA POLYGONATI with yellow rice wine
Acid-insoluble ash must not cross 1.5% in medicine materical crude slice.
Determination of moisture result is 8.91%~13.38%, and according to preliminary experiment measurement result, stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice moisture is surveyed
It is fixed to use《Chinese Pharmacopoeia》The method of four ruless of preparations of version in 2015 0832 second and the 4th method measurement result are basically identical, it is contemplated that
4th method complex operation and toluene have high toxicity, and this quality standard determines moisture in stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice using the second method,
Its content must not cross 15%.
Sealwort total starches assay result is 3.68%~8.20%,《Chinese Pharmacopoeia》The one regulation sealwort of version in 2015
Medicine materical crude slice Siberian solomonseal rhizome polysaccharide content must not be less than 4.0%, according to this result of study, and 3.5% must not be less than by being adjusted to Siberian solomonseal rhizome polysaccharide content.
Saponins of rhizoma polygonati measurement result is 0.78%~2.30%, in view of《Chinese Pharmacopoeia》Saponins of rhizoma polygonati content is not specified, this
Quality standard, which fixes tentatively saponins of rhizoma polygonati content, must not be less than 0.7%.
The quality evaluation of two integrated processing procedure finished products
This part content is mainly the wine processed according to above-mentioned quality standard research method to " integrated processing procedure "
Sealwort decoction piece quality standard is evaluated, the researching value and feasibility of preliminary identification new technology.
1. materials and methods
1.1 material
1.1.1 laboratory apparatus
Homogenous quantities research on standard part continuous item.
1.1.2 experiment reagent reagent
Cadmium yellow essence medicinal material (being provided by Hanzhong Lueyang sealwort medicinal material planting base), remaining is related with chapter 1 first segment
.
1.1.3 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice information
Stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice as prepared by embodiment 1, embodiment 2, embodiment 3, embodiment 4, control group is that commercially available wine is yellow
Essence.
1.2 method
1.2.1 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice character
Homogenous quantities research on standard part continuous item.
1.2.2 stir-baked RHIZOMA POLYGONATI with yellow rice wine differentiates
(1) microscopical characters
Homogenous quantities research on standard part continuous item.
(2) thin layer differentiates
Homogenous quantities research on standard part continuous item.
1.2.3 determination of extractives
Homogenous quantities research on standard part continuous item.
1.2.4 ash determination
Homogenous quantities research on standard part continuous item.
1.2.5 determination of moisture
Homogenous quantities research on standard part continuous item.
1.2.6 assay
(1) total starches assay
Homogenous quantities research on standard part continuous item.
(2) total saponin content is determined
Homogenous quantities research on standard part continuous item.
2. result
The character of 2.1 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
Embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice is in irregular sheet.Surface sepia, micro- glossy, tendon and vessel point is clear.Matter
It is relatively soft.Mouthful gustation sweet tea, smell it is micro- have yellow rice wine fragrance, with《Chinese Pharmacopoeia》(version in 2015) stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice recorded
Character is basically identical.
The discriminating of 2.2 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
2.2.1 micro-powder differentiates
Embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice micro-powder differentiates visible needle-like calcium oxalate crystal beam.
2.2.2 thin layer differentiates
According to the experimental method determined under " 1.2.2 (2) " item, using diosgenin as reference substance, 10 batches of stir-baked RHIZOMA POLYGONATI with yellow rice wine are drunk
Piece carries out indentification by TLC, the chromatographic behavior of embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice sample and the color of diosgenin reference substance
Spectrum behavior is consistent, and each spot can preferably realize separation.
2.3 determination of extractives
According to the 1.2.3 lower experimental methods determined, to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
Extract carry out assay, statistical analysis is carried out on the basis of experimental result, as a result such as table 7：
The determination of extractives result of table 7
2.4 ash determination
According to the 1.2.4 lower experimental methods determined, to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
Total ash, acid-insoluble ash content be measured, statistical analysis is carried out on the basis of experimental result, as a result such as table 8：
The ash measured result of table 8
2.5 determination of moisture
According to the 1.2.5 lower experimental methods determined, to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice
Moisture be measured, statistical analysis is carried out on the basis of experimental result, as a result such as table 9.
The determination of moisture result of table 9
2.6 assay
According to the 1.2.6.1 and 1.2.6.2 lower experimental method determined, to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control
The extract of group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice carries out assay, and statistical analysis is carried out on the basis of experimental result.
2.6.1 total starches assay
Each sample total reducing sugar measurement result such as table 10：
The total starches assay result of table 10
2.6.2 total saponin content is determined
Each sample total saposins measurement result such as table 11：
The total saponin content measurement result of table 11
3. discuss
(1) during thin layer differentiates, embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice sample are in same lamellae
Upper chromatographic behavior is consistent, and clear spot, separating degree is good.
(2) it is water-soluble extractives content to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice sample, dilute
Ethanol soluble extraction, n-butanol extract content, total starches, total saponin content, water content, total ash, acid-insoluble ash content
Meet the regulation that this research institute sets up quality standard continuous item, indices are superior to control group.
(3) the relative reservation at peak is mainly had to embodiment 1-4 stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice and control group stir-baked RHIZOMA POLYGONATI with yellow rice wine medicine materical crude slice sample
Time sets up the prescribed limit of quality standard continuous item in this research institute.
4. conclusion
The quality standard that the stir-baked RHIZOMA POLYGONATI with yellow rice wine prepared slice quality processed by " integrated processing procedure " meets the foundation of this research institute will
Ask, therefore think that " the integrated processing procedure " of the optimization of this research institute has feasibility.
Embodiment
The present invention is described in further details below by example, these examples are only used for illustrating the present invention, do not limit
The scope of the present invention processed.
The stir-baked RHIZOMA POLYGONATI with yellow rice wine of embodiment 1 integration Habitat producing and concocting method
Processing and processing step：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 3 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine, vexed profit 5 hours are sprayed on the sealwort sheet cut again；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 2 times repeatedly, produce.
The stir-baked RHIZOMA POLYGONATI with yellow rice wine of embodiment 2 integration Habitat producing and processing
Processing and processing step：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 10 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine, vexed profit 1 hour are sprayed on the sealwort sheet cut again；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 5 times repeatedly, produce.
The stir-baked RHIZOMA POLYGONATI with yellow rice wine of embodiment 3 integration Habitat producing and processing
Processing and processing step：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 5 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine is sprayed on the sealwort sheet cut again, vexed profit 2 hours, wherein yellow rice wine consumption are sealwort weight
20%；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 8 times repeatedly, produce.
The stir-baked RHIZOMA POLYGONATI with yellow rice wine of embodiment 4 integration Habitat producing and processing
Processing and processing step：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 5 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine is sprayed on the sealwort sheet cut again, vexed profit 2 hours, wherein yellow rice wine consumption are sealwort weight
20%；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steamed 12 hours, vexed 12 hours, room temperature airing 24 was small
When, " steam-vexed-dry in the air " 2 times repeatedly, produce.
The TLC Identification of the stir-baked RHIZOMA POLYGONATI with yellow rice wine of embodiment 5
The preparation of reference substance solution：Diosgenin reference substance is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol dissolving
And scale is settled to, shake up, concentration is made for 0.2mgmL-1Solution, produce；
The preparation of need testing solution：By sample comminution, 24 mesh sieves are crossed, test sample medicinal powder is obtained.Test sample medicinal powder 5.0g is weighed,
Put in flask, plus ethanol 50mL refluxing extraction 1h, suction filtration, filtrate adds hydrochloric acid 5mL to be heated to reflux 2h, after cooling, uses 40% hydrogen-oxygen
It is 7.0 to change sodium solution to be adjusted to pH, and water bath method solvent, residue heating water 40mL makes dissolving, and chlorination imitates extraction 3 times repeatedly, every time
30mL, combining extraction liquid, water-bath volatilizes chloroform, and residue adds methanol 10mL to make dissolving, shaken up, produces.
According to thin-layered chromatography experiment, draw reference substance solution and each 5 μ l of need testing solution are put in same silica G thin layer respectively
On plate, with cyclohexane-ethyl acetate-formic acid (4:1:0.1) mixed solution be development system, deploy, take out, dry, spray with
10% phosphomolybdic acid ethanol solution is developed the color, and clear spot is heated in 105 DEG C.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, is not departing from the technology of the present invention side's scope, when the technology contents using the disclosure above make a little change or are modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent variations and modification that above example is made, in the range of still falling within technical solution of the present invention.
Claims (6)
1. stir-baked RHIZOMA POLYGONATI with yellow rice wine integration Habitat producing and concocting method, it is characterised in that comprise the following steps：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 3-10 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine, vexed profit 1-5 hours are sprayed on the sealwort sheet cut again；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steaming 12 hours, vexed 12 hours, room temperature airing 24 hours,
" steam-vexed-dry in the air " 2-9 times repeatedly, produce.
2. the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine according to claim 1 and concocting method, it is characterised in that step (2) institute
It is 5 minutes to state sealwort sheet and put in boiling water the ironed time.
3. the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine according to claim 1 and concocting method, it is characterised in that step (3) institute
It is the 20% of sealwort weight to state yellow rice wine consumption, and the vexed profit time is 2 hours.
4. the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine according to claim 1 and concocting method, it is characterised in that step (4) institute
It is 2 times to state " steaming-vexed-dry in the air " number of times.
5. the integrated Habitat producing of stir-baked RHIZOMA POLYGONATI with yellow rice wine and concocting method according to claim 1-4, it is characterised in that including following
Step：
(1) the smart medicinal material of cadmium yellow is taken, impurity and dis-medicinal part is removed, cleans；
(2) clean cadmium yellow essence is put in boiling water and scalded 5 minutes, then directly cut into sheet, airing is half-dried；
(3) yellow rice wine is sprayed on the sealwort sheet cut again, vexed profit 2 hours, wherein yellow rice wine consumption are the 20% of sealwort weight；
(4) the vexed sealwort moistened of step (3) is placed in and steamed in container, steaming 12 hours, vexed 12 hours, room temperature airing 24 hours,
" steam-vexed-dry in the air " 2 times repeatedly, produce.
6. a kind of TLC Identification of stir-baked RHIZOMA POLYGONATI with yellow rice wine, it is characterised in that：
The preparation of reference substance solution：Diosgenin reference substance is taken, it is accurately weighed, put in 10mL measuring bottles, plus methanol dissolves and determined
Hold to scale, shake up, concentration is made for 0.2mgmL-1Solution, produce；
The preparation of need testing solution：By sample comminution, 24 mesh sieves are crossed, test sample medicinal powder is obtained.Test sample medicinal powder 5.0g is weighed, burning is put
In bottle, plus ethanol 50mL refluxing extraction 1h, suction filtration, filtrate adds hydrochloric acid 5mL to be heated to reflux 2h, after cooling, uses 40% sodium hydroxide
It is 7.0 that solution, which is adjusted to pH, water bath method solvent, and residue heating water 40mL makes dissolving, and chlorination is imitative to be extracted 3 times repeatedly, each 30mL,
Combining extraction liquid, water-bath volatilizes chloroform, and residue adds methanol 10mL to make dissolving, shaken up, produces.
According to thin-layered chromatography experiment, draw reference substance solution and each 5 μ l of need testing solution are put in same silica gel g thin-layer plate respectively
On, with cyclohexane-ethyl acetate-formic acid (4:1:0.1) mixed solution is development system, is deployed, and takes out, dries, and is sprayed with 10%
Phosphomolybdic acid ethanol solution is developed the color, and clear spot is heated in 105 DEG C.
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| CN108079187A (en) * | 2017-12-21 | 2018-05-29 | 贵州大学 | The place of production integration processing and concocting method of sealwort |
| CN108362788A (en) * | 2018-01-18 | 2018-08-03 | 成都中医药大学 | A kind of steamed sealwort Quality Detection analysis method |
| CN108770983A (en) * | 2018-05-22 | 2018-11-09 | 陕西师范大学 | A kind of production method of honey sealwort slice foodstuffs |
| CN109172739A (en) * | 2018-11-07 | 2019-01-11 | 陕西广济堂医药集团股份有限公司 | A kind of production method of stir-baked RHIZOMA POLYGONATI with yellow rice wine purification medicine materical crude slice |
| CN110343185B (en) * | 2019-07-11 | 2021-07-13 | 西北大学 | Wine-processed polygonatum polysaccharide and application thereof in regulating spleen deficiency and immune function |
| CN110343185A (en) * | 2019-07-11 | 2019-10-18 | 西北大学 | A kind of wine RHIZOMA POLYGONATI PREPARATA polysaccharide and its purposes in terms of spleen deficiency Immunity regulation |
| CN111195323A (en) * | 2020-01-17 | 2020-05-26 | 陕西中医药大学 | Rhizoma polygonati processing formula and technology |
| CN111743971A (en) * | 2020-06-05 | 2020-10-09 | 河南森源祥药材科技有限公司 | Novel processing method of rhizoma polygonati traditional Chinese medicine decoction pieces |
| CN111773312A (en) * | 2020-07-22 | 2020-10-16 | 西藏天虹科技股份有限责任公司 | Fine processing method of sealwort particles |
| CN111773312B (en) * | 2020-07-22 | 2021-11-16 | 西藏天虹科技股份有限责任公司 | Fine processing method of sealwort particles |
| CN113876887A (en) * | 2021-10-01 | 2022-01-04 | 浙江禾田兴生物科技有限公司 | Rhizoma polygonati processing method |
| CN115166121A (en) * | 2022-07-04 | 2022-10-11 | 陕西中医药大学 | Method for identifying different processed rhizoma polygonati products based on GC-IMS analysis of characteristic odor substances |
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