Summary of the invention
Technical problem to be solved by this invention is to provide a kind of concocting method of Rhizoma Arisaematis, the present invention is the improvement to existing processing procedure, while minimizing zest, elimination toxicity, reduce the toxic and side effects such as the aluminium ion caused owing to adopting existing concocting method exceeds standard, better ensure drug safety.
The present invention adopts quicklime to concoct Rhizoma Arisaematis, the mechanism of action is: in Rhizoma Arisaematis, main pungent component is needle-like calcium oxalate crystal, the superfine length of its crystal, needle point is sharp, and surface has agnail, and strong but pliable in texture resistance to mechanical power is strong, be difficult to fracture, intense stimulus can be produced to oral mucosa, oral cavity swelling can be caused once eat, time serious, also can cause dyspnea.This technique adopts quicklime to concoct Rhizoma Arisaematis, be needle-like calcium oxalate crystal in Rhizoma Arisaematis from outside to inside, little by little corroded to needle body by needle tip, come off, rust, rupture, thus lose zest and toxicity, to reach the effect of attenuation.Lime liquor decreases the residual of sulfur dioxide to a certain extent simultaneously.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of concocting method of Rhizoma Arisaematis, and its step is as follows:
1) get the Rhizoma Arisaematis that parts by weight are 80 ~ 120 parts, add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out;
2) get the caustic lime block that parts by weight are 5 ~ 15 parts, add water to submergence caustic lime block, furnishing suspension, sieves, and obtains lime liquor;
3) by 2) obtained lime liquor is added to 1) in the Rhizoma Arisaematis that soaked into, to submergence Rhizoma Arisaematis, stir evenly, infuse, dry, get product.
Concocting method advantage compared with traditional handicraft of Rhizoma Arisaematis of the present invention is: after concocting by the inventive method, the effective ingredient of Rhizoma Arisaematis does not reduce; Quicklime instead of Alumen and concocts Rhizoma Arisaematis, avoids in Alumen aluminum ions residual; After lime liquor is concocted, the sulfur dioxide minimizing that stove drying crude drug is residual; Quicklime convenient sources, economy is easy to get, and still can not be able to pollute as building materials coarse fodder after using.
On the basis of technique scheme, the present invention can also do following improvement.
Further, step 2) described in the temperature of water be 60 ~ 100 DEG C, be preferably 80 DEG C.
The beneficial effect of above-mentioned further scheme is adopted to be: fully to melt, caustic lime block;
Further, step 2) described in the aperture of sieving be 1 ~ 3mm, be preferably 1.5 ~ 2mm.
The beneficial effect of above-mentioned further scheme is adopted to be: sieve the lime particle that can remove and not melt and rock ballast etc., reduces the residual quantity of impurity in Rhizoma Arisaematis medical material, ensure drug safety;
Further, the time of infuse described in step 3) is 40 ~ 60 hours, is preferably 48 hours.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
Get 100g Rhizoma Arisaematis and add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out; Get 10g caustic lime block, add the water of 80 DEG C to submergence caustic lime block, furnishing suspension, crossing aperture is the sieve of 1.5mm, obtains lime liquor; Lime liquor is added in the Rhizoma Arisaematis soaked into, to submergence Rhizoma Arisaematis, stirs evenly, infuse 48 hours, dry, get product;
Embodiment 2
Get 80g Rhizoma Arisaematis and add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out; Get 5g caustic lime block, add the water of 60 DEG C to submergence caustic lime block, furnishing suspension, crossing aperture is the sieve of 2mm, obtains lime liquor; Lime liquor is added in the Rhizoma Arisaematis soaked into, to submergence Rhizoma Arisaematis, stirs evenly, infuse 48 hours, dry, get product;
Embodiment 3
Get 120g Rhizoma Arisaematis and add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out; Get 15g caustic lime block, add the water of 100 DEG C to submergence caustic lime block, furnishing suspension, crossing aperture is the sieve of 3mm, obtains lime liquor; Lime liquor is added in the Rhizoma Arisaematis soaked into, to submergence Rhizoma Arisaematis, stirs evenly, infuse 40 hours, dry, get product;
Embodiment 4
Get 100g Rhizoma Arisaematis and add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out; Get 10g caustic lime block, add the water of 60 DEG C to submergence caustic lime block, furnishing suspension, crossing aperture is the sieve of 1mm, obtains lime liquor; Lime liquor is added in the Rhizoma Arisaematis soaked into, to submergence Rhizoma Arisaematis, stirs evenly, infuse 60 hours, dry, get product;
Embodiment 5
Get 120g Rhizoma Arisaematis and add clear water to submergence Rhizoma Arisaematis, soak one day to thoroughly, pull out; Get 8g caustic lime block, add the water of 70 DEG C to submergence caustic lime block, furnishing suspension, crossing aperture is the sieve of 2.5mm, obtains lime liquor; Lime liquor is added in the Rhizoma Arisaematis soaked into, to submergence Rhizoma Arisaematis, stirs evenly, infuse 54 hours, dry, get product;
Experimental example 1
1, material
For examination material: Rhizoma Arisaematis, Rhizoma Arisaematis (processed)
Experimental facilities: UV-754 type ultraviolet/visible spectrophotometer (Shanghai Hong Ji instrument and equipment company limited), ultrasonic cleaning instrument
Main agents: quicklime, apigenin standard substance (Shanghai along vigorous biological engineering company limited, 201202), ethanol, triethylamine lot number:
2, method
2.1 quicklime concoct the screening study of Rhizoma Arisaematis process conditions
Adopt orthogonal experiment, according to the correlative factor affecting Calx concocted method, selecting the consumption (g) of the every 100g medical material of process of preparing Chinese medicine adjuvant quicklime used, soak time (h), melting the water temperature (DEG C) of adjuvant quicklime is three factors investigated, respectively get three levels, in table 1, adopt L
9(3
4) measure the mass fraction of Rhizoma Arisaematis calcium oxalate crystal growth in healthy needle under various condition.
Table 1 Calx concocted method orthogonal test factor level table
Oxalic acid calcium catalyst: the method is XH with reference to the author of Science Press's publication in 1981, " the photobiochemistry analytical method " of Bo Qinnuoke, P285 ~ 286,1ml HCL solution (1: 1) is added in the amalyzing substances precipitation in centrifuge tube, 15ml distilled water, stirs, puts into hot water (about 70 DEG C), periodic agitation 10min is then centrifugal.It is in the beaker of 50ml that solution pours volume into, and residue 0.1mol/L HCL reprocessing twice, use 10ml HCL at every turn, water-bath is heated 5min, will constantly stir simultaneously.At every turn with centrifugal after HCL process, and acid lixiviating solution is collected together.
In order to precipitate oxalic acid, in the acid solution of gained, add 2ml 25%CaCl
2solution, is heated to 70 ~ 80 DEG C, adds a methyl orange, then adds several NH
4oH concentrated solution is until occur muddy.Solution is under constantly stirring, and heating 1 ~ 2min, to make precipitation merge become crystallization, then continues heating, add several ammonia solutions until indicator becomes yellow.After this solution heats 5 ~ 10min again, and places 2h or a night.
Centrifugal after placing, pour out solution, and precipitation uses 10ml distilled water wash once.After pouring out the solution in precipitation, give in precipitation and add 10ml 1mol/L H
2sO
4solution stirs evenly, and while stirring, heat 3 ~ 5min in boiling water, centrifugal, solution is poured in titration bottle.Residue uses 10ml 1mol/L H again
2sO
4washing once, centrifugally to be poured solution in titration bottle into afterwards.Solution is heated to 60 ~ 70 DEG C, adds 1ml10%MnSO
4, then use 0.005mol/L MnSO
4it is rose-colored that solution is titrated to appearance, and no longer changed in several seconds.1ml 0.005mol/L MnSO
4be equivalent to 0.45mg H
2c
2o
4. with Ca
2+its content of the oxalic acid combined calculates according to the formula of water solublity salt-form oxalic acid amount in plant.In order to calculating oxalate calcium, acquired results is multiplied by 1.442.
Result: the optimum condition of Integrated Selection Calx concocted method, result as Table 2,3.
Table 2 orthogonal experiments
Table 3 analysis of variance table
2.2 measure the content that lime methods and CP method concoct effective ingredient after Rhizoma Arisaematis
Sample: the Rhizoma Arisaematis after the process of preparing Chinese medicine of lime method sample Example 1; CP method sample is the Rhizoma Arisaematis after concocting according to pharmacopeia " Pharmacopoeia of People's Republic of China (one) " (version in 2010) technique.
The preparation of reference substance solution: get apigenin (C
15h
10o
5) reference substance is appropriate, accurately weighed, add 60% ethanol and make the solution of every 1ml containing 12 μ g, to obtain final product.
The preparation of standard curve: precision measures reference substance solution 1ml, 2ml, 3ml, 4ml, 5ml, put in 10ml measuring bottle respectively, respectively add 60% ethanol to 5ml, add 1% triethylamine solution to scale, shake up, with corresponding reagent for blank, adopt the silica cuvette of 1cm, measure absorbance at the wavelength place of 400nm, corresponding absorbance A drawing standard curve, regression equation is y=0.159x+0.0092, R
2=0.9973, as shown in Figure 1.
Algoscopy: get two kinds of sample powder each (crossing No. four sieves) about 0.6g respectively, accurately weighed, put in tool plug conical flask, precision adds 60% ethanol 50ml, close plug, supersound process (power 250W, frequency 40kHz) 45 minutes, lets cool, weighed weight again, supply the weight of less loss with 60% ethanol, shake up, filter.Precision measures subsequent filtrate 5ml, puts in 10ml measuring bottle, the method under the preparation of sighting target directrix curve, from " 1% triethylamine solution ", measures absorbance in accordance with the law, reads the weight containing apigenin in need testing solution from standard curve, calculates, to obtain final product.This product is pressed dry product and is calculated, containing total flavones in apigenin (C
15h
10o
5).
Result: Rhizoma Arisaematis (processed) (CP method) general flavone content 0.095%, Rhizoma Arisaematis (processed) (lime method) general flavone content 0.103%.
2.3 measure the residual quantity that lime methods and CP method concoct sulfur dioxide after Rhizoma Arisaematis
Sample: the Rhizoma Arisaematis after the process of preparing Chinese medicine of lime method sample Example 1; CP method sample is the Rhizoma Arisaematis after concocting according to pharmacopeia " Pharmacopoeia of People's Republic of China (one) " (version in 2010) technique.
Algoscopy: the content measuring sulfur dioxide according to 2010 editions " Chinese Pharmacopoeia " annex IX U sulfur dioxide residual quantity algoscopys, device as shown in Figure 2, the each about 10g of sample thief powder, accurately weighed respectively, puts in two neck round-bottomed flasks, add water 300 ~ 400ml and 6mo1/L hydrochloric acid solution 10ml, connect scale separatory funnel, and import at the bottom of nitrogen to bottle, connect reflux condensing tube, connect airway at the E mouth place, upper end of condensing tube, airway is inserted bottom 250ml conical flask.125ml and starch indicator solution 1ml add water in conical flask as absorbing liquid, is placed on magnetic stirring apparatus and constantly stirs.Heat solution in two neck round-bottomed flasks to boiling, and start with iodine titration solution (0.01mol/L) titration after keeping micro-boiling about 3 minutes, continued for 20 seconds to blue or bluish violet and do not take off, and the result blank assay of titration is corrected.Calculate according to following formula:
In formula, A is the volume (ml) that test sample consumes iodine titration solution; B is the blank volume (ml) consuming iodine titration solution; C is iodine titration solution concentration 0.01mol/L; W is the weight (g) of test sample; 0.032 is the weight (g) of the suitable sulfur dioxide of every 1ml iodine titration solution (1mol/L).
Result: Rhizoma Arisaematis (processed) (CP method) sulfur content 165mg/kg, Rhizoma Arisaematis (processed) (lime method) sulfur content 76mg/kg.
3 sum up
3.1 pairs of lime methods concoct the summary of Rhizoma Arisaematis technique
According to the technique of " Pharmacopoeia of People's Republic of China (one) " (2010 editions) Rhizoma Arisaematis (processed), the mass fraction recording the needle-like calcium oxalate crystal of Rhizoma Arisaematis (processed) in CP method is 0.245%.When the Rhizoma Arisaematis calcium oxalate crystal growth in healthy needle mass fraction that Calx concocted method obtains is equal to or less than this value, namely think that Rhizoma Arisaematis (processed) now reaches drug safety.
The each factor of comprehensive analysis affects result to inspection target, and the optimised process being obtained lime method by direct analysis is A
2b
3c
1.Can find out that from variance analysis A, B, C factor has appreciable impact to inspection target, therefore select A
2(10g), B
3(48h), C
1(80 DEG C), therefore A
2b
3c
1for the optimised process of Calx concocted method, namely every 100g clean Rhizoma Arisaematis adjuvant Calx 10g, soaks 48 hours, opens quicklime by 80 DEG C of aquations.
The summary of active constituent content after 3.2 pairs of two kinds of methods process of preparing Chinese medicine Rhizoma Arisaematiss
Shown by above experimental result, the Rhizoma Arisaematis that lime method is concocted is compared with CP method Rhizoma Arisaematis (processed), and active constituent content does not reduce.
The summary of sulfur dioxide residual quantity after 3.3 pairs of two kinds of methods process of preparing Chinese medicine Rhizoma Arisaematiss
Fresh Rhizoma Arisaematis rots to go mouldy for preventing after gathering, and increases surperficial whiteness, dries, cause sulfur dioxide residue in medical material after generally adopting sulfur smoked.In Calx concocting process, sulfur dioxide is met water generation sulphoxylic acid and is reacted with the lime liquor generation acid-base neutralization of alkalescence, considerably reduces the residual of sulfur dioxide, ensure that drug safety.And do not use Alumen in quicklime concocting process, namely not containing Al
3+etc. harmful material.Therefore select lime method to concoct Rhizoma Arisaematis, Rhizoma Arisaematis quality can be improved, ensure drug safety.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.