The concocting method of Aconitum carmichaeli
Technical field
The invention belongs to the concocting method field of the prepared slices of Chinese crude drugs, and in particular to three kinds of concocting methods of Aconitum carmichaeli.
Background technology
Monkshood is the processed goods of the sub- root of the cohosh rhizome of Chinese monkshood (Aconitum carmichaelii Debx.), has and " returns
Sun rescues inverse first key medicine " title, clinical drug effect is remarkable.Monkshood is pungent, sweet, big heat;It is poisonous.The thoughts of returning home, kidney, the spleen channel.It has back
Sun rescues inverse, mends fire supporing yang, effect by wind-cold damp pathogen.For yang depletion collapse, cold weak pulse of limb, impotence, Gong Leng, trusted subordinate's crymodynia is empty
It is cold to vomit and diarrhoea, cold sensation of the genitalia oedema, numbness and ache of cold dampness.Its property is fiery and forthright fast, and ancient Chinese medicine doctor and herbal works all say monkshood " poisonous ", with it not
When easily there is serious toxic side effect, obvious cardiac toxic and neurotoxicity be mainly shown as in clinicing aspect, in addition in embryo
Also there is certain toxicity in terms of tire and kidney, therefore monkshood clinic is preferably processed and is used as medicine.
Monkshood successive dynasties concocting method has net system, cutting, frying, a several major classes of auxiliary material system, more than 18 kinds concocting methods, and Jiangxi is built
The concocting method of prosperous side monkshood is different from pharmacopeia and other concocting methods,《Help Chinese medicine preparation pandect in Jianchang》In to have recorded stewing attached
Piece, cloudy tag, positive tag, the concocting method of RADIX ACONITI LATERALIS PREPARATA, such as simmer tag:Choose salted aconite root to pour into bucket, add clear water, change daily
Water 2-3 times, changes before water and mixes up, and rinses 7-10 days;Drift to mouth tastes micro- salty to spend, and taking-up is dried;Lee is selected, one is built and encloses
Stove, ground is paved with thin chaff ash, and monkshood tail end is inserted in ash down, is drawn close to very close to each other;Quantitative ginger thin slice is taken, is covered
One layer of lid is in monkshood head;Tile two toilet paper on ginger splices, and tile one layer of chaff ash on paper, and tile a small amount of straw on ash;On straw
The dry chaff of the quantitative well sifted of tiling, is lighted a fire with straw from surrounding;About simmer 1-2 days processed, treat chaff ash cooling to the greatest extent, take out and simmer monkshood, to strike it
There is sound preferably;Monkshood will be simmered to be put into wooden rice steamer, a pot reclaimed water boiling is treated, water proof sits pot, and intense fire steams 8-10 hours;Steam to mouth taste without or
It is micro- to take out when having numb taste surface glossy, stand night day boil in a covered pot over a slow fire to sixty percent it is dry when cut into slices;Dry and do, weed out ash bits and produce.Either medicine
Allusion quotation is still《Help Chinese medicine preparation pandect in Jianchang》, have substantial amounts of indistinct fuzzy part to the concocting method of Chinese medicine, be not particularly suited for reality
Border is produced.
The content of the invention
In view of this, it is an object of the invention to provide the three of Aconitum carmichaeli kind concocting method, tag, the moon are specially simmered attached
Piece, positive tag.
The invention provides the concocting method that a kind of monkshood simmers tag, including:Used after rinsing net salinity per 100g salted aconite roots
10~15g gingers thin slice is simmered after 15~20h of system, steams 5~10h.
It is preferred that, the salted aconite root is to taste no saline taste by rinsing to mouth.
It is preferred that, the temperature for simmering system is 130~150 DEG C.
It is preferred that, the temperature steamed is 110~115 DEG C.
The invention provides a kind of concocting method of the cloudy tag of monkshood, including:Used after rinsing net salinity per 100g salted aconite roots
5~10h is steamed after 10~15h of the vexed profit of 10~20g ginger juices.
It is preferred that, the salted aconite root is to taste no saline taste by rinsing to mouth.
It is preferred that, described vexed profit is:The vexed profit in 20~30 DEG C, 65 ± 20%rh humidity environments.
It is preferred that, described steaming temperature is 110~115 DEG C.
The invention provides a kind of concocting method of the positive tag of monkshood, including:Rinsed per 100g salted aconite roots after net salinity
3~8min of frying in 15~30g sands.
It is preferred that, the temperature of the frying is 90~120 DEG C.
It is preferred that, the salted aconite root is to taste no saline taste by rinsing to mouth.
Technique effect
Compared with prior art, the concocting method for three kinds of Aconitum carmichaelis that the present invention is provided, is more suitable in actual production,
And after stewing tag of the invention, cloudy tag, positive attached film processing, the total of tag is simmered in the reduction of aconitine toxic component content
Alkaloid is the 56.25% of health product, and ester alkali content is the 12.89% of health product, and Content of Aconitine is the 20.35% of health product;
The total alkaloid content of cloudy tag is the 57.99% of health product, and ester alkali content is the 15.36% of health product, and Content of Aconitine is health product
22.08%;The total alkaloid content of positive tag is the 70.14% of health product, and ester alkali content is the 19.39% of health product, aconitine
Content is the 22.49% of health product, and the monkshood after processing also has certain synergistic effect to drug effect, and ethyl ether extract content substantially rises
Height, cloudy tag ethyl ether extract content is 3.65 times of health product, and positive tag ethyl ether extract content is 3.80 times of health product, is simmered attached
Piece ethyl ether extract content is 4.04 times of health product.
Embodiment
The invention provides the three of Aconitum carmichaeli kind concocting method, stewing tag, cloudy tag, positive tag are respectively obtained.
The invention provides the concocting method that a kind of monkshood simmers tag, including:Used after rinsing net salinity per 100g salted aconite roots
10~15g gingers thin slice is simmered after 15~20h of system, steams 5~10h.
Heretofore described salted aconite root, be able to can also make by oneself from commercially available;The preparation method of self-control salted aconite root includes:Choosing
Individual big, uniform mud monkshood, is cleaned, and the aqueous solution of the edible courage bar of immersion is stayed overnight, then adds salt, continues to soak, and daily remove is dried in the air
Shine, and gradually extend the drying time, until mass crystallization salt occurs in monkshood surface, constitution is hardened, and produces salted aconite root.
In the present invention, the net salinity of rinsing is defined by tasting no saline taste by rinsing to mouth.In the present invention, the rinsing
For (about 25 DEG C) at room temperature, salted aconite root is placed in container, clear water is added, water is changed daily, salinity is cleaned;It is preferred that, add
Clear water amount changes water there not to be salted aconite root to be defined, daily 2~3 times, and after the completion of cleaning, taking-up is dried, and ground is paved with thin chaff ash, will
Monkshood tail end is inserted in ash down, is drawn close to very close to each other;In the present invention, it is described to dry to remove surface in natural environment
Moisture, the thickness of the thin chaff ash is preferably 1cm ± 0.2cm.In the present invention, the effect of thin chaff ash is smouldered in stewing process processed,
Maintain the duration of temperature, it is to avoid medicinal material is contacted with naked light.
In the present invention, the thickness of the ginger thin slice is 0.3cm ± 0.1cm, and in the present invention, the ginger thin slice can
To weaken the toxicity of monkshood.
In the present invention, when the stewing is processed, the ginger thin slice is covered in monkshood head;The number of plies of the covering is preferably
One layer.
Described to simmer before system in the present invention, tile one layer of chaff ash on ginger thin slice upper berth toilet paper, toilet paper, and tiling is few on ash
The dry chaff that tiled on straw, straw is measured, is lighted a fire with straw from surrounding.It is preferred that, the chaff ash tiling thickness is 1~1.5cm;It is preferred that
, the dry chaff was No. 2 sieves, and the usage amount of the dry chaff is mainly degree can be ignited and cause lower floor's chaff ash burning.
In the present invention, toilet paper be in order on medicinal material plus chaff ash avoid medicinal material from being contacted with naked light;Chaff ash can smoulder simmering process processed, maintain
Temperature duration, it is to avoid medicinal material is contacted with naked light;Straw is fire-lighter, so that chaff ash burning can be caused to be degree.
In the present invention, described stewing temperature is preferably 130~150 DEG C, and the stewing time is preferably 16~18.5h,
More preferably 18h.The monkshood simmered after system, treats chaff ash cooling to the greatest extent, takes out, it is preferred that what the monkshood of taking-up struck has sound.
In the present invention, it is described steam in wooden rice steamer water proof steam, preferably after after boiling water in pot, water proof sits pot,
The temperature steamed is preferably 80~120 DEG C, more preferably 110~115 DEG C;The time steamed is 5~10h, excellent
Elect 7~9h, more preferably 8h as.
After the completion of being steamed in the present invention, take out the monkshood, stand night day boil in a covered pot over a slow fire to sixty percent it is dry when cut into slices, dry dry, weed out ash
Bits produce stewing tag;Stand night day stewing process is:Shine into surface no moisture but medicinal material is softer when cutting into slices, daytime paves
Dried in the air on level land, be placed in container and be capped or covered with gauze above in the evening;The thickness for simmering tag is 1~2mm.
The invention provides a kind of concocting method of the cloudy tag of monkshood, including:Used after rinsing net salinity per 100g salted aconite roots
5~10h is steamed after 10~15h of the vexed profit of 10~20g ginger juices.
In the present invention, the rinse method of the salted aconite root is identical with above-mentioned stewing tag.
In the present invention, the ginger juice is obtained by ginger squeezing, and specific preparation method is preferably included:By clean life
Ginger is smashed to pieces, is mixed with the water of ginger quality 15%, presses extracting juice.In the present invention, the number of times of the squeezing is preferably 2~5 times,
More preferably 4 times, the water of ginger weight 15% is added every time, merges juice, as ginger crush.
Ginger juice is mixed with the salted aconite root in the present invention, vexed profit is carried out to the salted aconite root;Preferably stir mixed
Close, preferred stirring to monkshood medicinal material surface has all contacted ginger juice;The consumption of the ginger juice is in terms of 100g salted aconite roots, preferably
For 10~20g, most preferably more preferably 12~16g, 15g.
It is preferred that, described vexed profit is preferably:The vexed profit in 20~30 DEG C, 65 ± 20%rh humidity sealed environments;It is described
The time of vexed profit is preferably 10~15h, more preferably 10.5~13h, most preferably 12h.
In the present invention, taking out the monkshood after vexed profit preferably enters in wooden rice steamer, treats a pot reclaimed water boiling, and water proof sits pot, continuous steaming
System, the temperature steamed is 110~115 DEG C, and the time steamed is 5~10h;6~8.5h is preferably steamed, more preferably
To steam 8h.
In the present invention, monkshood after steaming is taken out, and spreading for cooling is thinly sliced to seventy percent dry, dries to dry, produce monkshood cloudy
Tag, the thickness of cloudy tag is preferably 1~2mm.
The invention provides a kind of concocting method of the positive tag of monkshood, including:Rinsed per 100g salted aconite roots after net salinity
3~8min of frying in the net sand of 15~30g.
In the present invention, the rinse method of the salted aconite root is same simmers tag.It is preferred that, salted aconite root section, it is furthermore preferred that salt
Monkshood is cut into 1~3mm thin slices, most preferably, and salted aconite root is cut into 3mm thin slices.It is excellent after the salted aconite root shave in the present invention
Choosing, dry, it is furthermore preferred that drying hard to tag, quality becomes fragile.
In the present invention, the mass ratio of the salted aconite root and net sand is 100:10~30, more preferably 100:15~25, most
Preferably 100:20.In the present invention, the average grain diameter of the net sand is preferably 0.35~0.5mm.In the present invention, it is described to fry
System is preferably:Net sand is fried to 5-15min during fluent state with 100 DEG C of fire, the salted aconite root thin slice is poured into, keeps described net
Sand temperature carries out frying at 90~120 DEG C;The temperature of the net sand is more preferably maintained at 100 DEG C.Heretofore described frying
Time be preferably 3~8min, more preferably 5min.
In the present invention, after the completion of frying, monkshood thin slice is taken out, grey bits are weeded out, spreading for cooling produces the positive tag of monkshood.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.It is aobvious
So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the reality in the present invention
Example is applied, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made all belongs to
In the scope of protection of the invention.
Embodiment 1
Simmer the preparation of tag:Choose drift to mouth and taste micro- salty salted aconite root 100g for degree, taking-up is dried;Lee is selected, one is built
Stove is enclosed, ground is paved with thin chaff ash, monkshood tail end is inserted in ash down, is drawn close to very close to each other;Take thick 0.3cm ginger thin
Piece 12g, one layer of covering is in monkshood head;Tile two toilet paper on ginger splices, and tile one layer of chaff ash on paper, a small amount of rice of being tiled on ash
Grass;Tiled on straw and quantify the dry chaff of well sifted, lighted a fire with straw from surrounding;18h processed is simmered, chaff ash cooling to the greatest extent is treated, takes out and simmer monkshood, with
That strikes has sound preferably;Monkshood will be simmered to be put into wooden rice steamer, a pot reclaimed water boiling is treated, water proof sits pot, and 110 DEG C are steamed 8 hours, are taken out, and day spreads out
Night boil in a covered pot over a slow fire to sixty percent it is dry when be cut into 1mm thin slices;Dry and do, weed out ash bits and produce.
Embodiment 2
The preparation of cloudy tag:Get it filled material 100g, washes bleaching method with tag is simmered, takes out, dry, put in container, adds 15g lifes
Ginger is squeezed the juice, and mixes vexed profit 12h thoroughly, is taken out;Enter in wooden rice steamer, treat a pot reclaimed water boiling, water proof sits pot, and 110 DEG C of continuous steaming 8h take out;Spreading for cooling
It is dry to seventy percent, 3mm thin slices are cut into, dries to dry, produces.
Embodiment 3
The preparation of positive tag:Take drift to the light salted aconite root 100g for being cut into 3mm thin slices of mouth gustation, dry in the air to absolutely dry;Take 20g net
Sand is put into pot, is poured into tablet when being fried with 100 DEG C of fire to fluent state, is constantly stir-fried 5 minutes, takes out, weed out grey bits, spreading for cooling
Produce.
Embodiment 4
For tag made from embodiment 1~3, test sample about 4g is taken, it is accurately weighed, put 250~300ml conical flask
In, precision adds water 100ml, and close plug, cold soaking constantly shakes in first 6 hours, then stands 18 hours, is filtered rapidly with filter is dried,
Precision measures subsequent filtrate 20m l, puts and dries into the evaporating dish of constant weight, after being evaporated in water-bath, is dried 3 hours in 105 DEG C,
Put in drier and cool down 30 minutes, rapid accurately weighed weight.Unless otherwise specified, calculate water-soluble in test sample with dry product
The content (%) of extract.Determine the influence to monkshood water extraction content after processing:
Table 1:Process the influence to monkshood water extraction content
As can be seen from Table 1, after the method by the present invention is processed, water extraction content is significantly raised, cloudy tag water logging
Apparent extract is 1.487 times of health product, and positive tag water extraction content is 1.463 times of health product, simmers tag water extraction content
For 2.27 times of health product, active ingredient is significantly improved.
Embodiment 5
For tag made from embodiment 1~3, test sample (crossing No. four sieves) 2~5g is taken, it is accurately weighed, put five oxidations two
Dry 12 hours, put in apparatus,Soxhlet's in phosphorus drier, add diethyl ether appropriate, unless otherwise specified, be heated to reflux 8 hours, take
Ether solution, puts drying into the evaporating dish of constant weight, places, and flings to ether, it is small that residue puts drying 18 in phosphorus pentoxide desiccator
When, it is accurately weighed, 105 DEG C are slowly heated to, and dry to constant weight in 105 DEG C.Its less loss weight is volatility ether extract
Weight.Determine the influence to monkshood ethyl ether extract content after processing:
Table 2:Process the influence to monkshood ethyl ether extract content
As can be seen from Table 2, after the method by the present invention is processed, ethyl ether extract content is significantly raised, cloudy tag second
Ether extract content is 3.65 times of health product, and positive tag ethyl ether extract content is 3.80 times of health product, simmers tag ether and leaches
Thing content is 4.04 times of health product, and drug effect is significantly raised.
Embodiment 6
For tag made from embodiment 1~3, take sample liquid 20.0ml to be evaporated, residue is dissolved with a small amount of water, put a point liquid leakage
In bucket, pH=10~11 are adjusted with ammoniacal liquor, chloroform extracts 5 times (10,10,10,8,8ml), merges chloroform solution, reclaims chloroform, water-bath
Volatilize, residue ethanol 5.0ml dissolves, and precision adds sulfuric acid titrating solution (0.01mol/L) 15ml, water 15ml and methyl red and indicated
Liquid 3 is dripped, and yellow is titrated to sodium hydroxide titration liquid (0.02mo l/L), reads the amount of the NaOH solution of consumption, calculates total raw
The content of alkaloids (being detected as aconitine, ester alkali etc.).Determine the influence to Radix Aconiti Lateralis Preparata total alkaloids content after processing:
Table 3:Process the influence to Radix Aconiti Lateralis Preparata total alkaloids content
As can be seen from Table 3, after the method by the present invention is processed, total alkaloid content is substantially reduced in monkshood, cloudy attached
Piece total alkaloid content is the 56.25% of health product, and positive tag total alkaloid content is the 57.99% of health product, simmers tag always biological
Alkali content is the 70.14% of health product, toxicity reduction.
Embodiment 7
For tag made from embodiment 1~3, tag powder is taken to cross 60 mesh sieves about 1.0g, it is accurately weighed, put tool plug taper
In bottle, add diethyl ether 50ml and ammonia solution 4ml, and close plug shakes up, stood overnight.Ultrasonically treated 20min, filtration, the dregs of a decoction are washed with ether
Wash 3-4 times, each 5ml, filter, washing lotion merges with filtrate, and low temperature is evaporated.Residue adds 5% potassium hydroxide methanol solution 10ml, returns
1h is flowed, methanol is reclaimed, cooling, residue adds proper amount of methanol to dissolve, adjusts PH to 3-4 with concentrated hydrochloric acid about 0.8ml, is transferred to 5ml measuring bottles
In, plus mobile phase is to scale.Shake up, take subsequent filtrate as need testing solution.
Precision weighs benzoic acid reference substance 5.01mg and put in 25ml measuring bottles, plus methanol dissolves and dilute to scale, shakes up, then essence
The close 1ml that measures is put in 25ml measuring bottles, plus mobile phase is diluted to scale, shakes up, and produces benzoic acid reference substance solution.
Chromatographic column Phenomenex Luna C18 (150mm*4.6mm, 5 μm);Mobile phase methanol -0.05mol/L di(2-ethylhexyl)phosphates
Hydrogen potassium-acetic acid-isopropanol (67:173:4:4), 35 DEG C of column temperature, flow velocity 1.0ml/min sample sizes 5 μ l, Detection wavelength 230nm.Reason
3000 should be not less than by being calculated by plate number by benzoic acid peak.Under this chromatographic condition, reference substance solution, need testing solution are drawn respectively
Inject high performance liquid chromatograph.
The content of benzoic acid is calculated, coefficient 5.2877 is multiplied by, the content of total ester alkaloid is converted into terms of aconitine.Survey
Influence after fixed processing to monkshood ester alkali content:
Table 4:Process the influence to monkshood ester alkali content
As can be seen from Table 4, after the method by the present invention is processed, ester alkali content is substantially reduced in monkshood, cloudy tag ester
Alkali content is the 12.89% of health product, and positive tag ester alkali content is the 15.36% of health product, and it is health product to simmer tag ester alkali content
19.39%, toxicity reduction.
Embodiment 8
For tag made from embodiment 1~3, Waters BEH C18 chromatographic columns (2.1 × 50mm, 1.7 μm);Mobile phase
Acetonitrile:Tetrahydrofuran (25:15) it is mobile phase A, with 0.1mol/L ammonium acetate solutions (per 1000ml acetic acid 0.5ml on the rocks) for stream
Dynamic phase B, gradient elution program 0-8min (10%-14%A), 8-12min (14%-26%A), 12-15min (26%-35%A)
Flow velocity 0.3ml.min-1,35 DEG C of column temperature, Detection wavelength 235nm.
Precision weighs 3 kinds of reference substances in right amount, plus isopropanol-dichloromethane (1:1) mixed solution is made every 1ml and contained, new crow
Head the μ g of alkali 18.3, the μ g of 18 μ g Hypaconitines of aconitine 13.5 obtain mixed reference substance solution.
Sample powder (crossing No. three sieves) about 2g is taken, it is accurately weighed, put in conical flask with cover, ammonification test solution 3ml, precision is added
Isopropanol-ethyl acetate (1:1) mixed solution 50ml, weighed weight ultrasonically treated 30 minutes, is let cool, then weighed weight, with different
Propyl alcohol-ethyl acetate (1:1) mixed solution supplies the weight of less loss, shakes up, filtration.Precision measures subsequent filtrate 25ml, 40 DEG C with
Under solvent is recovered under reduced pressure to dry, residue precision adds isopropanol-dichloromethane (1:1) mixed solution 5ml dissolves, filtration, takes continuous
Filtrate, produces.Determine the influence to monkshood Content of Aconitine after processing:
Table 5:Process the influence to monkshood Content of Aconitine
As can be seen from Table 5, after the method by the present invention is processed, monkshood mesaconitine content is substantially reduced, cloudy tag
Content of Aconitine is the 20.35% of health product, and positive tag Content of Aconitine is the 22.08% of health product, simmers tag Content of Aconitine and is
The 22.49% of health product, toxicity reduction.
Embodiment 9
The LD of health product and each processed product50、Sx50And LD50Fiducial limit:
Table 6:The LD of health product and each processed product50、Sx50And LD50Fiducial limit
Medicine |
LD50 |
Sx50 |
LD50Fiducial limit |
Health product |
3.21 |
0.0296 |
2.80-3.66 |
Cloudy tag |
49.35 |
0.0321 |
42.70~57.04 |
Positive tag |
49.05 |
0.0240 |
44.01~54.65 |
Simmer tag |
52.99
|
0.0301
|
46.26~60.70
|
As seen from the above embodiment, after the method by the present invention is processed, cloudy tag, positive tag and the total biology for simmering tag
Alkali content, especially ester alkali, Content of Aconitine are significantly reduced, and ethyl ether extract content is significantly raised, it is seen then that by the present invention's
After processing, toxic component content reduction, active constituent content increases.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.