CN102406657A - Preparation method of montmorillonite preparations - Google Patents
Preparation method of montmorillonite preparations Download PDFInfo
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- CN102406657A CN102406657A CN201010291008XA CN201010291008A CN102406657A CN 102406657 A CN102406657 A CN 102406657A CN 201010291008X A CN201010291008X A CN 201010291008XA CN 201010291008 A CN201010291008 A CN 201010291008A CN 102406657 A CN102406657 A CN 102406657A
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Abstract
The invention relates to a preparation method of montmorillonite preparations, which is characterized in that the sum of any two impurity peak intensities in the X-ray powder diffraction pattern of adopted montmorillonite is not higher than the second characteristic peak of the montmorillonite; the drying loss is between 5 percent and 10.0 percent; the average grain diameter or the middle position diameter is not greater than 15 mum, the accumulated percentage of grains with the grain diameter smaller than 35 mum is not lower than 90 percent, and the specific surface area is not smaller than 8000 cm<2>/cm<3>; the absorption force is measured by a cation exchange volume method, and the cation exchange volume is 70 to 150 mmol/100g; and the silicon dioxide content is 55 percent to 65 percent, and the aluminum oxide content is 12 percent to 25 percent. The montmorillonite preparations have the advantages of high safety and good curative effect. Compared with the montmorillonite preparations on the market, the montmorillonite preparations have the controllable quality.
Description
Invention field
The present invention relates to a kind of method for preparing of Montmorillonitum preparation, belong to field of pharmaceutical technology.
Background technology
The Montmorillonitum preparation is through the proof of clinical practice for many years treatment diarrhoeal diseases determined curative effect, the medicine that toxic and side effects is little.But the Montmorillonitum quality of the pharmaceutical preparations of selling on the market now is on the low side, can not guarantee optimum curative effect.Trace it to its cause is that the raw materials used medicine quality of preparation Montmorillonitum medicine is on the low side.
The Montmorillonitum preparation of selling on the market now; The X-ray powder diffraction collection of illustrative plates of used Montmorillonitum raw material regulation in the method for preparing: " characteristic spectral line of Montmorillonitum is at about 1.5nm and 0.45nm place, and other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm) of Montmorillonitum in the collection of illustrative plates." such raw material might be inferior raw material.Montmorillonitum by bentonite exquisite and get, owing to the bentonitic minerogentic condition in the different places of production differs; Wherein the mineral of the content of Montmorillonitum and association thereof are also different; Be exactly same ore deposit point, the mineral species of its smectite content of different ore beds and association also has than big difference.The Montmorillonitum preparation of selling on the market now; Though the impurity peaks intensity in the X ray diffracting spectrum is not higher than second characteristic peak of Montmorillonitum; If but other impurity peaks intensity sums are greater than second characteristic peak of Montmorillonitum in the collection of illustrative plates; Then the amount of Montmorillonitum impurities also is many, prepares the Montmorillonitum preparation with such Montmorillonitum, has curative effect and potential safety hazard.
The Montmorillonitum preparation of selling on the market now, spectrophotography is used in the inspection of the absorption affinity of used Montmorillonitum raw material in the method for preparing; Measure the amount of absorption five water sulphuric acid strychnine, this method is measured absorption affinity specificity water-insoluble magnesium class mineral poor and the Montmorillonitum association and is seriously disturbed Montmorillonitum to adsorb the amount of five water sulphuric acid strychnine; Prepare the Montmorillonitum preparation with such Montmorillonitum; Absorption affinity is untrue, can not realize quality controllablely, and then can not guarantee the curative effect of preparation.
The Montmorillonitum preparation of selling on the market now, used Montmorillonitum raw material in the method for preparing, granularity is must not cross 1% greater than the particulate weight of 45um.The curative effect of Montmorillonitum is closely related with the fineness of the particles of its preparation, the granulometry that the thinner curative effect of granularity is good, so more, and scope is too wide, prepares the Montmorillonitum preparation with such Montmorillonitum, can not realize stable curative effect.
The Montmorillonitum preparation of selling on the market now; The content of used Montmorillonitum raw material is that " pressing dry product calculates; contain silicon dioxide (SiO2) and should not be less than 50.0%, trioxygen-containingization two aluminum (Al2O3) should not be less than 10.0% " such Montmorillonitum raw material contains more and the dirt Montmorillonitum association in the method for preparing.Dioxide-containing silica has only 83.9% of theoretical value, and aluminium sesquioxide content has only 43.6% of theoretical value, and by this standard, the kaolinite or the illite that contain a small amount of quartz also meet content requirement; Zeolite also can meet content requirement; Bentonite also can meet content requirement.Prepare the Montmorillonitum preparation with such Montmorillonitum, can not guarantee the curative effect of preparation.
The Montmorillonitum preparation of selling on the market now, the moisture of used Montmorillonitum raw material is in the method for preparing: " get these article 2.0g, be dried to constant weight at 105 ℃, subtract weight loss and must not cross 10.0%." there is defective in the moisture Control of this Montmorillonitum raw material.Three kinds of moisture are arranged in the Montmorillonitum: its content of liquid Free water on surface is indefinite, and is relevant with the degree of drying of Montmorillonitum.This water just can evaporate under the condition of a little higher than room temperature; The interlayer adsorbed water, the density of interlayer adsorbed water, the aqueous water that viscosity is more usual are big, begin during greater than 100 ℃ to overflow, and purify basically about 300 ℃; Participate in constituting the water of Montmorillonitum lattice, dehydration temperaturre is different different because of Montmorillonitum constitutes, and a Yin Dynasty deviates from more more than 500 ℃, purify basically about 800 ℃.Montmorillonitum has considerable interlayer adsorbed water to overflow under 105 ℃ temperature, dehydration product at this moment, and most can also rehydrations the recovery, but rehydration thing and original structure are incomplete same; Having few part to cause the montmorillonite layer chip architecture " to subside " can not rehydration recover.If the used Montmorillonitum raw material of Montmorillonitum preparation has only the upper limit, there is not lower limit, possibly cause the Montmorillonitum overdrying, cause Montmorillonitum intermediary water vagus escape, cause the montmorillonite layer chip architecture to destroy, thereby affect the treatment.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing Montmorillonitum preparation, a kind of method for preparing of high-quality Montmorillonitum preparation is provided, to guarantee the optimum curative effect of Montmorillonitum preparation.
The objective of the invention is to realize like this, a kind of method for preparing of Montmorillonitum preparation prepares the Montmorillonitum preparation with the Montmorillonitum crude drug that meets following technical standard:
Natural bentonite is got through washing refining being processed into by Montmorillonitum system, is hydrated aluminium silicate salt.
[character] Montmorillonitum crude drug is a canescence or for yellow fine powder, adds the abnormal smells from the patient that water has clay after moistening, and color burn; Almost insoluble in water, diluted acid or alkali hydroxide test solution.
[discriminating] (1) gets the Montmorillonitum crude drug and each 0.5g of calcium fluoride puts in the same platinum crucible, and it is moistening to add sulphuric acid 1ml, covers crucible with the surface plate that adds 1 in water, can slowly heat like necessity, and the adularescent colloid generates on the water droplet surface.
(2) it is an amount of to get the Montmorillonitum crude drug, measures according to Chinese Pharmacopoeia X ray powder art diffraction approach, and the X ray diffracting spectrum of Montmorillonitum should be consistent with the Montmorillonitum collection of illustrative plates of international powder crystal X-ray diffraction archives; Other impurity peaks intensity must not be higher than second characteristic peak (about 0.45nm) of Montmorillonitum in the collection of illustrative plates.
(3) solution under the aluminium sesquioxide assay item should show the identification of aluminum salt.
[inspection] PH is got Montmorillonitum crude drug 0.20g, adds water 20ml, puts on the boiling water bath heating after 2-3 minute, puts coldly, filters, and gets filtrating and measures by 2005 editions two appendix VI H of Chinese Pharmacopoeia, and pH value should be 5.0-9.0.
Chloride is got Montmorillonitum crude drug 0.20g, adds 1 in water 25ml and nitric acid, boils 5 minutes, filters, and gets filtrating according to two appendix VIII of Chinese Pharmacopoeia version in 2005 A inspection, and the contrast liquor ratio of processing with standard chloride solution 5.0ml must not denseer (0.025%).
Carbonate is got Montmorillonitum crude drug 0.2g, puts in the test tube, adds water 2ml and makes it suspendible; The acetum 2ml that adds 2mol/L, rapidly with the close plug of stopper with the glass bend pipe, slowly heating; Escaping gas is imported in the calcium hydroxide test solution, must not the adularescent deposition produce.
Solute is got Montmorillonitum crude drug 2.0g in the water, adds water 50mL, boils 5 minutes, and adds water and be adjusted to 50mL, puts coldly, and after filtering with filter paper, the microporous membrane of reuse 0.45 μ m filters, and the filtrating water bath method is dried to constant weight at 105 ℃, leaves over residue and must not cross 14mg.
Loss on drying is got the Montmorillonitum crude drug, is dried to constant weight at 105 ℃, subtracts weight loss between 5-10.0%;
Granularity is measured granularity with Particle Size Analyzer, attaches IX E third party according to Chinese Pharmacopoeia 2010 editions and measures, and mean diameter or meso-position radius must not be greater than 15um, and particle diameter is not less than 90% less than the particulate accumulative total percentage rate of 35um, and specific surface area must not be less than 8000cm2/cm3.
Heavy metal is got Montmorillonitum crude drug 4.0g, adds acetate buffer 4ml and the water 46ml of pH3.5, boils; Put coldly, add water and make into 50ml, filter; Get filtrating 25ml,, contain heavy metal and must not cross 10/1000000ths according to the inspection of 2005 editions appendix VIII of Chinese Pharmacopoeia H, first method.
Arsenic salt is got Montmorillonitum crude drug 1.0g, adds hydrochloric acid 5ml and water 23ml, and according to the inspection of Chinese Pharmacopoeia version appendix in 2005 VIII J first method, arsenic salt must not cross 2/1000000ths.
Swelling degree is got Montmorillonitum crude drug 1.0g in the 100ml band plug graduated cylinder that adds 40ml, adds water to 75ml scale place again.The jam-pack stopper shakes up 3 minutes, and sample is fully scattered, and adds the 1mol hydrochloric acid solution of 25ml, and jolting 5 minutes was left standstill 24 hours, read the scale value at precipitate interface, was swelling degree; Swelling degree should be 10-25ml.
Absorption affinity is measured with the cation exchange capacity method, and cation exchange capacity should be at 70-150mmol/100g;
Microorganism is limited the quantity of and is got the Montmorillonitum crude drug, according to microbial limit detection method (2005 editions two appendix XI J of Chinese Pharmacopoeia) test, and should be up to specification.
[assay] Montmorillonitum crude drug is pressed dry product and is calculated, and contains silicon dioxide (SiO2) and should be 55%-65%, and trioxygen-containingization two aluminum (Al2O3) should be 12%-25%.
Assay method is following: aluminium sesquioxide is got the about 1.0g of Montmorillonitum crude drug, and accurate the title decides, and puts in the porcelain dish, adds sulphuric acid 6ml and nitric acid 10ml respectively; Treat effect fully, put evaporate to dryness in the sand bath, put coldly, add dilute sulfuric acid 30ml; Boil, upper strata liquid filters through ashless filter paper with decantation, and with hot wash 3 times, washing liquid filters residue in the lump with decantation; With on the residue dislocation filter paper, use hot wash at last, residue is waited to do silicon dioxide and is used; Filtrating merges, and places the 100ml measuring bottle, puts and is chilled to room temperature, and thin up shakes up to scale; Precision is measured 20ml, adds ammonia solution and is neutralized to and just separates out deposition, drips dilute sulfuric acid to deposition more just till the dissolving; Add acetic acid-ammonium acetate buffer (pH6.0) 10ml, the accurate again Calcium Disodium Versenate volumetric solution 25ml that adds 0.05mol/L boiled 3-5 minute; Put and be chilled to room temperature, add xylenol orange indicator solution 1ml, with the zinc volumetric solution titration of 0.05mol/L; Change redness into from yellow to solution, and titration results is proofreaied and correct with blank assay; The aluminium sesquioxide of the suitable 2.549mg of Calcium Disodium Versenate volumetric solution of every 1ml0.05mol/L;
Silicon dioxide is got above-mentioned residue and is put in the platinum crucible together with filter paper, and drying was descended blazing 2 hours at 800 ℃, put cold; The accurate title, decide, and adds sulphuric acid 0.2ml and ethanol 2ml and make test sample moistening fully, adds Fluohydric acid. 6ml, puts 100-300 ℃ of evaporation; Put coldly during near doing, repeated hydrogenation fluoric acid 6ml makes test sample moistening fully, puts 100-300 ℃ and is evaporated to gas and eliminates, slowly be warming up to 800 ℃ blazing 1 hour; Put coldly, accurate claim surely, subtract the weight of mistake, be and contain silica weight in the test sample.
The method for preparing of a kind of Montmorillonitum preparation of the present invention; Used Montmorillonitum is measured according to x-ray powder diffraction; The record collection of illustrative plates; The X ray diffracting spectrum of test sample should be consistent with the Montmorillonitum collection of illustrative plates of international powder crystal X-ray diffraction archives, and any two impurity peaks intensity sums must not be higher than second characteristic peak of Montmorillonitum in the collection of illustrative plates.
Particle Size Analyzer of the present invention is laser diffractometry Particle Size Analyzer or sedimentation Particle Size Analyzer.Laser diffractometry is Fraunhofer diffraction again; Approximate dead ahead scattering of light; Laser scattering method and low angle laser light scattering.
The method for preparing of a kind of Montmorillonitum preparation of the present invention; Measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum mean diameter or meso-position radius must not be greater than 15um with stirring method; Particle diameter less than 35um must not be less than 90%, and specific surface area must not be less than 8000cm
2/ cm
3
The mean diameter of pressed powder, meso-position radius, accumulative total percentage rate reach 90% particle diameter, and specific surface area equigranular parameter index connects each other, and the quality of control product also can be selected wherein one.This Montmorillonitum grain size parameter index can be reduced to: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with stirring method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 35um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 15um; Or used Montmorillonitum specific surface area must not be less than 8000cm
2/ cm
3
The method for preparing of a kind of Montmorillonitum preparation of the present invention; Measuring granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine, is to be disperse medium with water, disperses with stirring method; Used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 20um; Particle diameter must not be less than 99% less than the particulate accumulative total percentage rate of 30um, and mean diameter or meso-position radius must not be greater than 10um, and specific surface area must not be less than 9000cm
2/ cm
3
This Montmorillonitum grain size parameter index can be reduced to: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with stirring method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 20um; Or used Montmorillonitum particle diameter must not be less than 99% less than the particulate accumulative total percentage rate of 30um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 10um; Or used Montmorillonitum specific surface area must not be less than 9000cm2/cm3.
The method for preparing of a kind of Montmorillonitum preparation of the present invention; Measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 15um with ultransonic method; Mean diameter or meso-position radius must not be greater than 5um, and specific surface area must not be less than 15000cm
2/ cm
3
This Montmorillonitum grain size parameter index can be reduced to: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with ultransonic method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 15um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 5um; Or used Montmorillonitum specific surface area must not be less than 15000cm
2/ cm
3
The method for preparing of a kind of Montmorillonitum preparation of the present invention; Measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 8um with ultransonic method; Mean diameter or meso-position radius must not be greater than 3um, and specific surface area must not be less than 25000cm2/cm3.
This Montmorillonitum grain size parameter index can be reduced to: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with ultransonic method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 8um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 3um; Or used Montmorillonitum specific surface area must not be less than 25000cm
2/ cm
3
The absorption affinity of Montmorillonitum derives from the imbalance of its internal charge.In the Montmorillonitum Si-O tetrahedral sheet, quaternary Si is sometimes by tervalent Al replacement, in the Al-O octahedral sheet; Tervalent Al is sometimes by the Mg of bivalence replacement, and this just causes positive charge not enough, and negative charge is superfluous; The negative charge of this surplus is compensated by the cation of absorption on the crystal layer surface; When having water to exist, the compensating cation on crystal layer surface is called exchange absorption easily by other cation exchange.The Montmorillonitum cation exch ange adsorption has following characteristics: (1) jack per line ion exchanges each other, and cation in Montmorillonitum unit's crystal layer and the exchange interaction between the cation in the solution are stoichiometric reactions, meet mass action law; (2) etc. electric weight (or equivalent) is intercoursed, the cation that the Montmorillonitum surface exchange is come out with equated by the cationic electric weight (or equivalent) of Montmorillonitum absorption, intercourse like 1 Ca2+ and 2 Na+; (3) cationic exchange and absorption are reversible.According to the ion exchange absorption characteristics of Montmorillonitum, being adsorbed agent can be in water or alcoholic solution, to dissociate positive ionic chemical compound.These chemical compounds comprise that ammonium acetate, ammonium chloride, methylene blue, quinine sulfate, berberine, betanin, barium chloride etc. can dissociate positive ionic chemical compound in water or alcoholic solution.Absorption affinity is represented with mmol/100g, also can convert g/100g, g/g, and the absorption of promptly every 100g Montmorillonitum is adsorbed the mmol number of agent, the absorption of every 100g Montmorillonitum and is adsorbed the g number that the g number of agent, the absorption of every 1g Montmorillonitum are adsorbed agent.
The method for preparing of a kind of Montmorillonitum preparation of the present invention, used Montmorillonitum loss on drying are to get the Montmorillonitum crude drug, are dried to constant weight at 105 ℃, subtract weight loss between 5-10.0%.
The method for preparing of a kind of Montmorillonitum preparation of the present invention, used Montmorillonitum are pressed dry product and are calculated, and contain silicon dioxide (SiO2) and should be 55%-65%, and trioxygen-containingization two aluminum (Al2O3) should be 12%-25%;
Montmorillonitum preparation of the present invention comprises Montmorillonitum powder, smectite turbid liquor, montmorillonite gelling, Montmorillonitum sheet, Montmorillonitum capsule, Montmorillonitum granule.
The method for preparing of the various preparations of Montmorillonitum preparation of the present invention is to use method for preparing preparation commonly used on the galenic pharmacy.
Crude drug with meeting above-mentioned technical standard prepares the Montmorillonitum preparation, and safe, curative effect is better than the Montmorillonitum preparation that gone on the market, quality controllable.
Announce Test Example below, further specify beneficial effect of the present invention.
The Montmorillonitum powder of testing the present invention preparation compares with commercially available Montmorillonitum powder treatment diarrheal clinical efficacy and safety.
Purpose: estimate Montmorillonitum powder treatment diarrheal clinical efficacy and safety with the present invention's preparation.
Method: adopt at random double blinding, the diffusing medicine parallel check experiment design of commercially available Montmorillonitum.21 routine acute diarrhea patients have been observed altogether, test group 11 examples wherein, matched group 10 examples, 3 days courses of treatment.22 routine chronic diarrhea patients, test group 11 examples wherein, matched group 11 examples, 7 days courses of treatment.
Result: 1. effectiveness: the Montmorillonitum powder treatment acute diarrhea effective percentage 100% of the present invention's preparation, chronic diarrhea effective percentage 90.91%; The commercially available Montmorillonitum of matched group looses and treats acute diarrhea effective percentage 85.00%, chronic diarrhea effective percentage 76.91%.Two groups relatively, significant difference.
2. safety: the test group adverse reaction rate is 4.55% after the medication, and matched group is 4.76%, two group and compares the difference not statistically significant.Two groups aspect lab testing, all do not see the abnormal change that clinical meaning is arranged before and after each item index treatment.
Conclusion: clinical trial shows that it is effective and safe that Montmorillonitum powder that the present invention prepares is treated acute and chronic diarrhoea, and its curative effect is better than commercially available Montmorillonitum powder.
Test used Montmorillonitum raw material of two the present invention and commercially available Montmorillonitum raw material granularity relatively.
Sample: the used Montmorillonitum raw material of the present invention (self-control)
Commercially available Montmorillonitum raw material (purchasing) in certain company
Test condition (meeting two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine): laser particle size analyzer, instrument model Winner2000ZD; The pretreatment does not have; Dispersal pattern, wet method is disperseed; Ultrasound wave does not have; Mixing speed, 300 rev/mins; Software version; V1.0; The focal length of lens, 50; Optical concentration, 1.0-2.5; The photon diffusion models of using, Mie scattering; Complex index, real part 1.51, imaginary part 0.01; The fitting parameter that diffraction ring is resolved, squared differences.
Test result: the used Montmorillonitum raw material of the present invention, particle diameter is less than the particulate accumulative total percentage rate 98.37% of 35um, specific surface area 12272.67cm
2/ cm
3, meso-position radius 6.5lum, mean diameter 8.53um.
Commercially available Montmorillonitum raw material, particle diameter is less than the particulate accumulative total percentage rate 63.25% of 35um, specific surface area 4750.69cm
2/ cm
3Meso-position radius 26.50um, mean diameter 31.42um.
Test three usefulness ammonium acetates are measured the used Montmorillonitum absorption affinity of the present invention
Take by weighing 2g Montmorillonitum sample, be placed in the acid filtrating bucket of 105mL, under the condition of finding time, the use pH value is 7 the neutral NH of 1mol/L
4Ac drip washing drenches liquid with the suction bottle reception of 500ml, till drip washing to the reaction with the no calcium of calcon-carboxylic acid inspection; Reuse 80% ethanol drip washing; Remove the NH4Ac of retention, sample in the filter funnel moved in the Kai Shi bottle, water with sample all towards the Kai Shi bottle; Making in the bottle last volume is 50mL, in bottle, adds several small porcelain rings, prevents bumping.The magnesia magma 10ml that adds 100g/L makes mixture be alkalescence, distills immediately according to the operation of measuring total nitrogen content then, reserves NH in the liquid
3Boric acid 20ml with 60g/L absorbs, and distillation finishes the back with 0.02mol/L salt acidometric titration absorption liquid, calculates the Montmorillonitum absorption affinity.Cation exchange capacity is 140mmol/100g as a result, and promptly used Montmorillonitum absorption affinity is 140mmol/100g.
Test four-function ammonium chloride is measured the used Montmorillonitum absorption affinity of the present invention
Take by weighing 1g Montmorillonitum sample, put in the centrifuge tube, add 20ml50% ethanol, on magnetic stirring apparatus, stirred 5 minutes, take off centrifugally, clear liquid discards.Add 50ml0.5N ammonium chloride-50% alcoholic solution, on magnetic stirring apparatus, stirred 30 minutes, take off centrifugal; Clear liquid moves in the l00ml volumetric flask, and precipitate is with 95% washing with alcohol 2 times, 20ml at every turn; Clear liquid discards, and precipitate moves in the Kelvin bottle, and water is rare to 50ml; Add 10 milliliters of 10% magnesium oxide suspensions, make mixture be alkalescence, distill immediately according to the operation of measuring total nitrogen content; NH4 in the distillate absorbs with the saturated boric acid of 20ml, with the salt acidometric titration absorption liquid of 0.5N, calculates the Montmorillonitum absorption affinity after distillation finishes.Cation exchange capacity is 71mmol/100g as a result, and promptly used Montmorillonitum absorption affinity is 71mmol/100g.。
Test five usefulness methylene blues are measured the used Montmorillonitum absorption affinity of the present invention
Take by weighing 1g Montmorillonitum sample, place in the conical beaker, add the 50ml distilled water; Make its moistening in advance, adding concentration then is 1% sodium pyrophosphate solution 20ml, rock evenly after; Heated and boiled 5 minutes on electric furnace is cooled to room temperature again, and using burette to call in concentration is 0.2% methylene blue solution.During titration, can add for the first time and estimate about 2/3rds of methylene blue solution amount, splash into 1-2ml later at every turn.The method of check terminal point is to rock about 30 seconds after dripping methylene blue solution at every turn; Be stained with an examination section on the middling speed quantitative filter paper with Glass rod, observe the halo that around the dark blue color dot of central authorities, has or not appearance what is said or talked about blueness, when the end occurs; Continue to drip methylene blue solution; So repeatable operation till the blue halo of the tangible what is said or talked about of appearance, arrives test endpoint.The titer of methylene blue solution is the blue amount of suction of this sample at this moment.Calculating the Montmorillonitum cation exchange capacity is 150mmol/100g, and promptly used Montmorillonitum absorption affinity is 150mmol/100g.
Test six usefulness quinine sulfate are measured the used Montmorillonitum absorption affinity of the present invention
Adopt the absorption affinity of fluorescent spectrophotometric determination Montmorillonitum to quinine sulfate, calculating the Montmorillonitum cation exchange capacity is 100mmol/100g, and promptly used Montmorillonitum absorption affinity is 100mmol/100g.
Test seven usefulness berberines are measured the used Montmorillonitum absorption affinity of the present invention
Adopt the absorption affinity of high effective liquid chromatography for measuring Montmorillonitum to berberine sulphate, calculating the Montmorillonitum cation exchange capacity is 135mmol/100g, and promptly used Montmorillonitum absorption affinity is 1135mmol/100g.
Test eight garden beet alkali and measure the used Montmorillonitum absorption affinity of the present invention
Adopt the absorption affinity of colorimetric method for determining Montmorillonitum to betanin, calculating the Montmorillonitum cation exchange capacity is 95mmol/100g, and promptly used Montmorillonitum absorption affinity is 95mmol/100g.
The specific embodiment
Further specify the present invention below in conjunction with embodiment.
The raw materials used medicine Montmorillonitum of embodiment 1 chemical examination the present invention,
Test condition (meeting two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine): laser particle size analyzer, instrument model Winner2000ZD; The pretreatment does not have; Dispersal pattern, wet method is disperseed; Ultrasound wave, ultrasonic 60s; Mixing speed, 300 rev/mins; Software version; V1.0; The focal length of lens, 50; Optical concentration, 1.0-2.5; The photon diffusion models of using, Mie scattering; Complex index, real part 1.51, imaginary part 0.01; The fitting parameter that diffraction ring is resolved, squared differences.Result such as following table:
The raw materials used medicine Montmorillonitum chemical examination of the present invention report
Judge: the result is up to specification
Embodiment 2
With the qualified Montmorillonitum feedstock production Montmorillonitum powder of embodiment 1 chemical examination, take by weighing Montmorillonitum 300g, glucose 74.9g, saccharin sodium 0.7g, vanillin 0.4g, fully mixing is distributed into every bag of powder that contains Montmorillonitum 3g.
Embodiment 3
With the qualified Montmorillonitum feedstock production smectite turbid liquor of embodiment 1 chemical examination; Take by weighing Montmorillonitum 300g, glucose 74.9g, saccharin sodium 0.7g, vanillin 0.4g, sodium benzoate 0.5g adds water to 3000ml; Stir, promptly get 10% smectite turbid liquor.
Embodiment 4
With the qualified Montmorillonitum feedstock production montmorillonite gelling of embodiment 1 chemical examination, take by weighing Montmorillonitum 300g, glucose 74.9g, saccharin sodium 0.7g, vanillin 0.4g, sodium benzoate 0.5g adds water to 1500ml, stirs, and promptly gets 20% montmorillonite gelling.
Embodiment 5
With the qualified Montmorillonitum feedstock production Montmorillonitum tablet of embodiment 1 chemical examination, take by weighing Montmorillonitum 300g, glucose 74.9g, saccharin sodium 0.7g, vanillin 0.4g, methylcellulose 10, fully mixing; Wet granulation, drying, granulate; It is an amount of to add lubricant, mixing, and tabletting promptly gets.
Embodiment 6
With the qualified Montmorillonitum feedstock production Montmorillonitum capsule of embodiment 1 chemical examination, take by weighing Montmorillonitum 300g, wet granulation, drying, granulate, the adding lubricant is an amount of, incapsulates promptly to get.
Embodiment 7
With the qualified Montmorillonitum feedstock production Montmorillonitum granule of embodiment 1 chemical examination, take by weighing Montmorillonitum 300g, glucose 74.9g, saccharin sodium 0.7g, vanillin 0.4g, abundant mixing, wet granulation, drying, granulate promptly gets.
Claims (12)
1. the method for preparing of a Montmorillonitum preparation is characterized in that preparing the Montmorillonitum preparation with the Montmorillonitum crude drug that meets following technical standard:
Natural bentonite is got through washing refining being processed into by Montmorillonitum system, is hydrated aluminium silicate salt;
[character] Montmorillonitum crude drug is a canescence or for yellow fine powder, adds the abnormal smells from the patient that water has clay after moistening, and color burn; Almost insoluble in water, diluted acid or alkali hydroxide test solution;
[discriminating] (1) gets the Montmorillonitum crude drug and each 0.5g of calcium fluoride puts in the same platinum crucible, and it is moistening to add sulphuric acid 1ml, covers crucible with the surface plate that adds 1 in water, can slowly heat like necessity, and the adularescent colloid generates on the water droplet surface;
(2) it is an amount of to get the Montmorillonitum crude drug; X-ray powder diffraction is measured; The X ray diffracting spectrum of Montmorillonitum should be consistent with the Montmorillonitum collection of illustrative plates of international powder crystal X-ray diffraction archives, and other impurity peaks intensity must not be higher than the characteristic peak at about 0.45nm place of Montmorillonitum in the collection of illustrative plates;
(3) solution under the aluminium sesquioxide assay item should show the identification of aluminum salt;
[inspection] PH is got Montmorillonitum crude drug 0.20g, adds water 20ml, puts on the boiling water bath heating after 2-3 minute, puts coldly, filters, and gets filtrating and measures by 2005 editions two appendix VI H of Chinese Pharmacopoeia, and pH value should be 5.0-9.0;
Chloride is got Montmorillonitum crude drug 0.20g, adds 1 in water 25ml and nitric acid, boils 5 minutes; Filter; Get filtrating according to two appendix VIII of Chinese Pharmacopoeia version in 2005 A inspection, with concentration be the contrast liquor ratio processed of 0.025% standard chloride solution 5.0ml, must not be denseer;
Carbonate is got Montmorillonitum crude drug 0.2g, puts in the test tube, adds water 2ml and makes it suspendible; The acetum 2ml that adds 2mol/L, rapidly with the close plug of stopper with the glass bend pipe, slowly heating; Escaping gas is imported in the calcium hydroxide test solution, must not the adularescent deposition produce;
Solute is got Montmorillonitum crude drug 2.0g in the water, adds water 50mL, boils 5 minutes, and adds water and be adjusted to 50mL, puts coldly, and after filtering with filter paper, the microporous membrane of reuse 0.45 μ m filters, and the filtrating water bath method is dried to constant weight at 105 ℃, leaves over residue and must not cross 14mg;
Loss on drying is got the Montmorillonitum crude drug, is dried to constant weight at 105 ℃, subtracts weight loss between 5-10%;
Granularity attaches IX E third party mensuration according to Chinese Pharmacopoeia 2010 editions, and mean diameter or meso-position radius must not be greater than 15um, and particle diameter is not less than 90% less than the particulate accumulative total percentage rate of 35um, and specific surface area must not be less than 8000cm
2/ cm
3
Heavy metal is got Montmorillonitum crude drug 4.0g, adds acetate buffer 4ml and the water 46ml of pH3.5, boils; Put coldly, add water and make into 50ml, filter; Get filtrating 25ml,, contain heavy metal and must not cross 10/1000000ths according to the inspection of 2005 editions appendix VIII of Chinese Pharmacopoeia H, first method;
Arsenic salt is got Montmorillonitum crude drug 1.0g, adds hydrochloric acid 5ml and water 23ml, and according to the inspection of Chinese Pharmacopoeia version appendix in 2005 VIII J first method, arsenic salt must not cross 2/1000000ths;
Swelling degree is got Montmorillonitum crude drug 1.0g in the 100ml band plug graduated cylinder that adds 40ml, adds water to 75ml scale place again.The jam-pack stopper shakes up 3 minutes, and sample is fully scattered, and adds the 1mol hydrochloric acid solution of 25ml, and jolting 5 minutes was left standstill 24 hours, read the scale value at precipitate interface, was swelling degree; Swelling degree should be 10-25ml;
Absorption affinity is measured with the cation exchange capacity method, and cation exchange capacity should be at 70-150mmol/100g;
Microorganism is limited the quantity of and is got the Montmorillonitum crude drug, according to the test of 2005 editions two appendix XI J of Chinese Pharmacopoeia microbial limit detection method, and should be up to specification;
[assay] Montmorillonitum crude drug is pressed dry product and is calculated, and contains silicon dioxide and should be 55%-65%, and trioxygen-containingization two aluminum should be 12%-25%.
2. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1; It is characterized in that: measure according to the Chinese Pharmacopoeia x-ray powder diffraction; The X ray diffracting spectrum of used Montmorillonitum should be consistent with the Montmorillonitum collection of illustrative plates of international powder crystal X-ray diffraction archives, and any two impurity peaks intensity sums must not be higher than second characteristic peak of Montmorillonitum in the collection of illustrative plates.
3. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum mean diameter or meso-position radius must not be greater than 15um with stirring method; Particle diameter less than 35um must not be less than 90%, and specific surface area must not be less than 8000cm
2/ cm
3
4. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1 or claim 3; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with stirring method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 35um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 15um; Or used Montmorillonitum specific surface area must not be less than 8000cm
2/ cm
3
5. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1 or claim 3; It is characterized in that: measuring granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine, is to be disperse medium with water, disperses with stirring method; Used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 20um; Particle diameter must not be less than 99% less than the particulate accumulative total percentage rate of 30um, and mean diameter or meso-position radius must not be greater than 10um, and specific surface area must not be less than 9000cm
2/ cm
3
6. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1 or claim 3 or claim 5; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with stirring method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 20um; Or used Montmorillonitum particle diameter must not be less than 99% less than the particulate accumulative total percentage rate of 30um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 10um; Or used Montmorillonitum specific surface area must not be less than 9000cm
2/ cm
3
7. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 15um with ultransonic method; Mean diameter or meso-position radius must not be greater than 5um, and specific surface area must not be less than 15000cm
2/ cm
3
8. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1 or claim 7; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water; Disperse with ultransonic method, used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 15um; Or used Montmorillonitum mean diameter or meso-position radius must not be greater than 5um; Or used Montmorillonitum specific surface area must not be less than 15000cm
2/ cm
3
9. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1 or claim 7; It is characterized in that: measure granularity according to two appendix IV of Chinese Pharmacopoeia version in 2010 E three therapeutic methods of traditional Chinese medicine; Be to be disperse medium with water, disperse that used Montmorillonitum particle diameter must not be less than 90% less than the particulate accumulative total percentage rate of 8um with ultransonic method; Mean diameter or meso-position radius must not be greater than 3um, and specific surface area must not be less than 25000cm
2/ cm
3
10. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1, it is characterized in that: measure absorption affinity with the cation exchange capacity method, cation exchange capacity is between 70-150mmol/100g; It is used that to be adsorbed agent be in water or alcoholic solution, to dissociate positive ionic chemical compound.
11. according to the method for preparing of a kind of Montmorillonitum preparation of claim 1, it is characterized in that: used Montmorillonitum loss on drying is to get the Montmorillonitum crude drug, is dried to constant weight at 105 ℃, subtracts weight loss between 5-10.0%.
12. the method for preparing according to a kind of Montmorillonitum preparation of claim 1 is characterized in that: used Montmorillonitum is pressed dry product and is calculated, and containing silicon dioxide is 55%-65%, and trioxygen-containingization two aluminum are 12%-25%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102636419A (en) * | 2012-04-27 | 2012-08-15 | 济南康众医药科技开发有限公司 | Method for checking granularity of montmorillonite |
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| CN101477068A (en) * | 2009-01-20 | 2009-07-08 | 济南康众医药科技开发有限公司 | Medicinal smectite content measuring standard |
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| CN105454288A (en) * | 2016-01-11 | 2016-04-06 | 济南康众医药科技开发有限公司 | Pesticide prepared from montmorillonite and used for preventing and controlling crop diseases |
| CN105454287A (en) * | 2016-01-11 | 2016-04-06 | 济南康众医药科技开发有限公司 | Pesticide prepared from montmorillonite and using method thereof |
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| CN105669270A (en) * | 2016-01-11 | 2016-06-15 | 济南康众医药科技开发有限公司 | Anti-continuous cropping fertilizer |
| CN110794052A (en) * | 2019-10-30 | 2020-02-14 | 刘圣梅 | Method for measuring adsorption capacity of montmorillonite |
| CN110793926A (en) * | 2019-10-30 | 2020-02-14 | 刘圣梅 | Method for measuring adsorption capacity of montmorillonite |
| CN110823881A (en) * | 2019-10-30 | 2020-02-21 | 刘圣梅 | Method for measuring montmorillonite adsorption force by using berberine sulfate |
| CN112386607A (en) * | 2020-11-17 | 2021-02-23 | 华润三九(唐山)药业有限公司 | Preparation method of montmorillonite particles |
| CN112794336A (en) * | 2021-01-29 | 2021-05-14 | 海南海力制药有限公司 | Purification method of montmorillonite, montmorillonite powder and preparation method thereof |
| CN117205334A (en) * | 2023-10-09 | 2023-12-12 | 青岛市中心医院 | Berberine-loaded montmorillonite composite material and preparation method and application thereof |
| CN117205334B (en) * | 2023-10-09 | 2024-05-24 | 青岛市中心医院 | Berberine-loaded montmorillonite composite material and preparation method and application thereof |
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