CN101477068A - Medicinal smectite content measuring standard - Google Patents
Medicinal smectite content measuring standard Download PDFInfo
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- CN101477068A CN101477068A CNA200910014003XA CN200910014003A CN101477068A CN 101477068 A CN101477068 A CN 101477068A CN A200910014003X A CNA200910014003X A CN A200910014003XA CN 200910014003 A CN200910014003 A CN 200910014003A CN 101477068 A CN101477068 A CN 101477068A
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Abstract
The invention discloses a standard for determining the content of medicinal montmorillonite, and in particular relates to a standard for controlling the content of silicon dioxide and aluminium sesquioxide in a quality standard of medicinal montmorillonite with pertinence. The standard is characterized in that the content standard of silicon dioxide and aluminium sesquioxide is as follows: the content of montmorillonite needs to be between 95.0 and 105.0 percent; according to the calculation of dry matter, the content of silicon dioxide (SiO2) needs to be between 55 and 65 percent; and the content of aluminium sesquioxide (Al2O3) needs to be between 12 and 22 percent.
Description
Invention field
The present invention relates to the medicinal smectite medicinal smectite content measuring standard, belong to drug standards technical field.
Background technology
Smectite is through the proof of clinical practice for many years treatment diarrhoeal diseases determined curative effect, the medicine that toxic and side effect is little.Existing medicinal smectite quality standard regulation: press dry product and calculate, contain silicon dioxide (SiO
2) should be no less than 50%, trioxygen-containingization two aluminium (Al
2O
3) should be no less than 10%.
Smectite is bentonitic principal ingredient, is made by bentonitic clay washing impurity elimination, and the principal ingredient that constitutes smectite is silicon dioxide and alundum (Al.Because bentonitic clay becomes the ore deposit parent rock different with mineralization characteristics and smectite preparation technology thereof, medicinal smectite often has impurity such as the oxide, solubility salt of associated mineral illite, smalite, halloysite, malthacite, zeolite, quartz, opaline, feldspar, pyrite, iron to exist except that smectite.
Silicon dioxide, alundum (Al weight content number percent according to bibliographical information and smectite associated mineral are respectively:
Mineral name dioxide-containing silica alundum (Al content
Illite 45.18% 34.66%
Smalite 47.51% 38.22%
Malthacite 20-30% 29-50%
Zeolite 65-71% 11-13%
Quartzy principal ingredient is a silicon dioxide
The opaline principal ingredient is a silicon dioxide
Desirable montmorillonite formula is: (Si
8) Al
3.34Mg
0.66) O
20(OH)
4
↓
(1/2Ca，Na)0.66
(1/2Ca, Na) expression is used for compensating the interlayer exchangeable cations of the positive charge loss that different valency ion exchange causes in the formula.The content that calculates its silicon dioxide according to following formula is 59.58%, and the content of alundum (Al is 22.96%, SiO
2/ Al
2O
3Weight percent value ratio is 2.59.
Published the Geology Publishing House in 1994, has put down in writing in " Chinese bentonitic clay mineral deposit and Application and Development " book that Yao Daokun writes, and the bentonitic clay silicon dioxide in the different places of production of China, the content of alundum (Al see Table 1.
The bentonitic clay silicon dioxide in the different places of production of table 1, the content of alundum (Al
According to above-mentioned bibliographical information, in bentonitic clay, when containing associated minerals such as illite, smalite, malthacite except that smectite, the silicon dioxide content test value is just less than 59.58%, and alundum (Al assay value is just greater than 22.96%.In bentonitic clay, when containing associated minerals such as zeolite, quartz, opaline except that smectite, the silicon dioxide content test value is just greater than 59.58%, and alundum (Al assay value is just less than 22.96%.In bentonitic clay, when containing non-silicon dioxide, alundum (Al mineral except that smectite, silicon dioxide, alundum (Al content all are lower than theoretical value.
The medicinal smectite quality standard should be controlled silicon dioxide, alundum (Al content lower bound, controls silicon dioxide, the high limit of alundum (Al content again, could effectively control the quality of medicinal smectite, and then guarantee the curative effect of smectite.But also there is not report at present at the control criterion of medicinal smectite and associated mineral impurity thereof.
The defective of silicon dioxide, alundum (Al content standard is in the existing medicinal smectite quality standard, is not at the control of medicinal smectite and associated mineral impurity thereof, can not reflect smectite content.The silicon dioxide of stipulating in the standard, alundum (Al content had not both met theoretical value, did not meet the practical measurement value yet; Dioxide-containing silica has only 83.9% of theoretical value, and alundum (Al content has only 43.6% of theoretical value, and by this standard, the smalite or the illite that contain a small amount of quartz also can be qualified; Zeolite also can meet the medicinal smectite quality standard; Bentonitic clay also can meet medicinal standard.Such standard can not be controlled drug quality effectively, and then can influence clinical efficacy.
The objective of the invention is,, provide a kind of new standard that can control the medicinal smectite quality effectively for overcoming the defective of silicon dioxide, alundum (Al content standard in the existing medicinal smectite quality standard.
In fact, the present invention relates to silicon dioxide in the medicinal smectite quality standard, alundum (Al content standard.
Summary of the invention
The invention discloses medicinal smectite content measuring standard, be specifically related to a kind of silicon dioxide in the medicinal smectite quality standard, alundum (Al content standard controlled targetedly.
Silicon dioxide involved in the present invention, alundum (Al content standard are: contain smectite and should be 95.0%-105.0%, press dry product and calculate, contain silicon dioxide (SiO
2) should be 55%-65%, trioxygen-containingization two aluminium (Al
2O
3) should be 12%-22%.
Medicinal smectite content measuring standard involved in the present invention, silicon dioxide content test method are gelatin method or hydrofluorite method, and the alundum (Al content assaying method is titrimetry or atomic absorption spectrography (AAS).
The gelatin method is measured silicon dioxide, titration measuring alundum (Al:
It is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 0.5g, the accurate title, decide, and puts in the platinum crucible, adds 0.5g sodium carbonate and 0.5g sal tartari, stir evenly, slowly heat up, descended blazing 3 hours cooling at 800 ℃, gradation adds watery hydrochloric acid 50ml altogether, stirring is dissolved residue fully and is transferred to the 250ml beaker, and crucible washs with the low amounts of water gradation, and washing lotion is incorporated in the beaker, after heating boils off the solution of about 1/2 volume, put coldly, add 20ml hydrochloric acid and 1ml 2% gelatin solution, in 60～70 ℃ of water bath heat preservations 10 minutes, stir constantly, filtered while hot, and use the hot wash container, collection filtrate and washing lotion are standby; Then filter paper and residue are moved in the crucible of ignition to constant weight,, calculate, promptly get dioxide-containing silica at 1100 ℃ of ignition to constant weight;
Get above-mentioned filtrate and washing lotion, put in the 250ml measuring bottle, thin up is to scale, shake up, precision pipettes 75ml, adding ammonia solution is neutralized to and just separates out white precipitate, drip watery hydrochloric acid to white precipitate again and just dissolve, filter, get filtrate and add acetic acid-ammonium damping fluid (pH6.0) 10ml, add Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 5 minutes, and put and be chilled to room temperature, add xylenol orange indicator solution 1ml, transfer to solution with zinc vs (0.05mol/L) and just become redness, add sodium fluoride 0.4g then, boiled 2 minutes, put cold after, transfer to solution with zinc vs (0.05mol/L) and change redness into by Huang, every 1ml zinc vs (0.05mol/L) is the Al of 2.549mg quite
2O3 calculates, and promptly gets alundum (Al content.
Titration measuring alundum (Al, hydrofluorite are measured silicon dioxide:
It is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 1.0g, the accurate title, decide, and puts in the porcelain dish, adds sulfuric acid 6ml and nitric acid 10ml respectively, the effect for the treatment of fully, is put evaporate to dryness in the sand bath, puts cold, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last with on the residue dislocation filter paper with decantation, use hot wash, residue is waited to do silicon dioxide and is used; Filtrate 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, adding ammonia solution is neutralized to and just separates out precipitation, drip dilute sulfuric acid again and extremely precipitate till the just dissolving, add acetic acid-ammonium acetate buffer (pH6.0) 10ml, precision adds Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 3～5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, with zinc vs (0.05mol/L) titration, change redness into from yellow to solution, and titration results is proofreaied and correct with blank test.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is the Al203 of 2.549mg quite, calculates, and promptly gets alundum (Al content;
Get above-mentioned residue together with filter paper put with platinum alloy crucible in, drying, 800 ℃ blazing 2 hours down, put cold, accurate claim fixed.With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness, 800 ℃ blazing 5 minutes, put coldly, accurate claim surely, subtract the weight of mistake, be and contain SiO in the test sample
2Weight is calculated, and promptly gets dioxide-containing silica.
The hydrofluorite method is measured silicon dioxide, atomic absorption spectroscopy determination alundum (Al:
It is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 0.25g, and accurate the title decides, put in the platinum crucible, be heated to 900 ℃, blazing 2 hours, cooling, add sulfuric acid 0.2ml and ethanol 2ml, make test sample moistening fully, add hydrofluorite 6ml, put 100 ℃ of-300 ℃ of evaporations, adding hydrofluorite 6ml when closely dried, continue to be evaporated to gas and eliminate, slowly be warming up to 900 ℃, blazing 1 hour, cooling, accurate claim surely, the weight of twice blazing gained poor is and contains SiO in the test sample
2Amount, calculate, promptly get dioxide-containing silica;
The preparation of alundum (Al reference substance solution: get Lu 1.0g, the accurate title, decide, and puts in the 1000ml measuring bottle, adds hydrochloric acid 10ml and water 10ml, after the dissolving, adds water to scale, shakes up, promptly;
The preparation of need testing solution: it is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 0.25g, the accurate title, decide, and puts in the platinum crucible, adds anhydrous lithium metaborate 1g, mix, slowly be warming up to 1100 ℃, blazing 15 minutes, put cold, crucible is placed the beaker of the rare nitric acid of 250ml (1 → 20), add rare nitric acid (1 → 20) 50ml again, Tianjin there is not crucible, crucible is put in the magnetic stirring, heating is stirred to dissolving fully, filters rapidly, filtrate is put in the 200ml measuring bottle, wash crucible and filter with water, washing lotion is incorporated in the measuring bottle, adds water to scale, shake up, promptly;
Measure alundum (Al content: precision is measured alundum (Al reference substance solution 0.5,1.0,2.0ml puts respectively in the 100ml measuring bottle, respectively add 1% sodium chloride solution 20ml, add water to scale, shake up, each reference substance solution and the need testing solution of dilution are shone atomic absorption spectrophotometry (two appendix IV of Chinese Pharmacopoeia version in 2005 D content determination, first method), measure at 309nm wavelength place, calculate, promptly get alundum (Al content.
Medicinal smectite content measuring standard of the present invention, silicon dioxide, alundum (Al content also can be used for the quality inspection of smectite preparation, calculate with smectite net content in the smectite preparation to get final product.
Smectite preparation of the present invention comprises clinical formulations commonly used such as powder, tablet, capsule, granule, supensoid agent, gel, dispersing tablet.
The present invention compared with prior art, has following advantage: at medicinal smectite and associated mineral impurity thereof, silicon dioxide, alundum (Al content range of control have been formulated, can control the content of medicinal smectite impurity effectively, guarantee the quality of medicinal smectite and preparation thereof, and then guarantee the clinical efficacy of smectite.
The relevant technologies terminological interpretation that the present invention relates to.The implication of " acetic acid-ammonium damping fluid (pH6.0) " is acetic acid-ammonium damping fluid of pH6.0.This is the method that the national drug standards are represented various damping fluid ph values; The implication of " Calcium Disodium Versenate vs (0.05mol/L) " is: " concentration through precision calibration is 0.05mol/L Calcium Disodium Versenate solution ", this is the regulation in the Chinese Pharmacopoeia note on the use.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
Get bentonitic clay and pulverize, make X ray diffracting spectrum, carry out qualitative and quantitative analysis, the result also contains impurity such as illite and smalite except that smectite about 30%, and it is an amount of to get this product, and 105 ℃ are dried to constant weight, take by weighing about 0.5g, the accurate title, decide, and puts in the platinum crucible, adds 0.5g sodium carbonate and 0.5g sal tartari, stir evenly, slowly heat up, descended blazing 3 hours cooling at 800 ℃, gradation adds watery hydrochloric acid 50ml altogether, stirring is dissolved residue fully and is transferred to the 250ml beaker, and crucible washs with the low amounts of water gradation, and washing lotion is incorporated in the beaker, after heating boils off the solution of about 1/2 volume, put coldly, add 20ml hydrochloric acid and 1ml2% gelatin solution, in 60～70 ℃ of water bath heat preservations 10 minutes, stir constantly, filtered while hot, and use the hot wash container, collection filtrate and washing lotion are standby; Then filter paper and residue are moved in the crucible of ignition to constant weight,, calculate at 1100 ℃ of ignition to constant weight, dioxide-containing silica be 53%.
Get above-mentioned filtrate and washing lotion, put in the 250ml measuring bottle, thin up shakes up to scale.Precision pipettes 75ml.Adding ammonia solution is neutralized to and just separates out white precipitate, dripping watery hydrochloric acid to white precipitate more just dissolves, filter, get filtrate and add acetic acid-ammonium damping fluid (pH6.0) 10ml, add Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, transfer to solution with zinc vs (0.05mol/L) and just become redness, add sodium fluoride 0.4g then, boiled 2 minutes, put cold after, transfer to solution with zinc vs (0.05mol/L) and change redness into by Huang, every 1ml zinc vs (0.05mol/L) is the Al of 2.549mg quite
2O3 calculates, and gets alundum (Al content 15%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, defective.
Embodiment 2
It is an amount of to get zeolite, and 105 ℃ are dried to constant weight, take by weighing about 1.0g, the accurate title, decide, and puts in the porcelain dish, adds sulfuric acid 6ml and nitric acid 10ml respectively, the effect for the treatment of fully, is put evaporate to dryness in the sand bath, puts cold, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, with hot wash 3 times, washing lotion filters residue in the lump, at last with on the residue dislocation filter paper with decantation, use hot wash, residue is waited to do silicon dioxide and is used; Filtrate 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, adding ammonia solution is neutralized to and just separates out precipitation, drip dilute sulfuric acid again and extremely precipitate till the just dissolving, add acetic acid-ammonium acetate buffer (pH6.0) 10ml, precision adds Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 3～5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, with zinc vs (0.05mol/L) titration, change redness into from yellow to solution, and titration results is proofreaied and correct with blank test.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is the Al of 2.549mg quite
2O
3, calculate, get alundum (Al content 10%;
Get above-mentioned residue together with filter paper put with platinum alloy crucible in, drying, 800 ℃ blazing 2 hours down, put cold, accurate claim fixed.With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness, 800 ℃ blazing 5 minutes, put coldly, accurate claim surely, subtract the weight of mistake, be and contain SiO in the test sample
2Weight is calculated, and gets dioxide-containing silica 66%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, defective.
Embodiment 3
Get bentonitic clay, after the water that adds 8 times of amounts fully stirs, placed 24 hours, draw the top suspension, discard bottom impurity, filter, filter cake is pulverized in dry below 105 ℃, makes X ray diffracting spectrum, carry out qualitative and quantitative analysis, smectite content is 98% as a result, takes by weighing an amount of, 105 ℃ are dried to constant weight, take by weighing about 0.25g, and accurate the title decides, put in the platinum crucible, be heated to 900 ℃, blazing 2 hours, cooling adds sulfuric acid 0.2ml and ethanol 2ml, makes test sample moistening fully, add hydrofluorite 6ml, put 100 ℃ of-300 ℃ of evaporations, adding hydrofluorite 6ml when closely dried, continue to be evaporated to gas and eliminate, slowly be warming up to 900 ℃, blazing 1 hour, cooling, the accurate title, decide, the weight of twice blazing gained poor is and contains SiO in the test sample
2Amount, calculate, dioxide-containing silica 55%;
The preparation of alundum (Al reference substance solution: get aluminium 1.0g, the accurate title, decide, and puts in the 1000ml measuring bottle, adds hydrochloric acid 10ml and water 10ml, after the dissolving, adds water to scale, shakes up, promptly;
The preparation of need testing solution: it is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 0.25g, the accurate title, decide, and puts in the platinum crucible, adds anhydrous lithium metaborate 1g, mix, slowly be warming up to 1100 ℃, blazing 15 minutes, put cold, crucible is placed the beaker of the rare nitric acid of 250ml (1 → 20), add rare nitric acid (1 → 20) 50ml again, Tianjin there is not crucible, crucible is put in the magnetic stirring, heating is stirred to dissolving fully, filters rapidly, filtrate is put in the 200ml measuring bottle, wash crucible and filter with water, washing lotion is incorporated in the measuring bottle, adds water to scale, shake up, promptly;
Measure alundum (Al content: precision is measured alundum (Al reference substance solution 0.5,1.0,2.0ml puts respectively in the 100ml measuring bottle, respectively add 1% sodium chloride solution 20ml, add water to scale, shake up, each reference substance solution and the need testing solution of dilution are shone atomic absorption spectrophotometry (two appendix IVD of Chinese Pharmacopoeia version in 2005 content determination, first method), measure at 309nm wavelength place, calculate, get alundum (Al content 16.7%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, qualified.
Embodiment 4
Get bentonitic clay, after the water that adds 8 times of amounts fully stirs, placed 24 hours, draw the top suspension, discard bottom impurity, filter, filter cake is pulverized in dry below 105 ℃, makes X ray diffracting spectrum, carry out qualitative and quantitative analysis, smectite content is 95% as a result, and it is an amount of to get this product, 105 ℃ are dried to constant weight, take by weighing about 0.5g, and accurate the title decides, put in the platinum crucible, add 0.5g sodium carbonate and 0.5g sal tartari, stir evenly, slowly heat up, descended blazing 3 hours at 800 ℃, cooling, gradation add watery hydrochloric acid 50ml altogether, and stirring is dissolved residue fully and transferred to the 250ml beaker, crucible washs with the low amounts of water gradation, washing lotion is incorporated in the beaker, after heating boils off the solution of about 1/2 volume, puts cold, add 20ml hydrochloric acid and 1ml2% gelatin solution, in 60～70 ℃ of water bath heat preservations 10 minutes, stir filtered while hot constantly, and use the hot wash container, collection filtrate and washing lotion are standby; Then filter paper and residue are moved in the crucible of ignition to constant weight,, calculate at 1100 ℃ of ignition to constant weight, dioxide-containing silica be 64.6%.
Get above-mentioned filtrate and washing lotion, put in the 250ml measuring bottle, thin up shakes up to scale.Precision pipettes 75ml.Adding ammonia solution is neutralized to and just separates out white precipitate, dripping watery hydrochloric acid to white precipitate more just dissolves, filter, get filtrate and add acetic acid-ammonium damping fluid (pH6.0) 10ml, add Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, transfer to solution with zinc vs (0.05mol/L) and just become redness, add sodium fluoride 0.4g then, boiled 2 minutes, put cold after, transfer to solution with zinc vs (0.05mol/L) and change redness into by Huang, every 1ml zinc vs (0.05mol/L) is the Al of 2.549mg quite
2O3 calculates, and gets alundum (Al content 12.4%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, qualified.
Embodiment 5
Get commercially available smectite and loose, add washing and remove auxiliary material, in dry below 105 ℃, pulverize, make X ray diffracting spectrum, carry out qualitative and quantitative analysis, smectite content is 90% as a result, contains quartz in addition, α-cristobalite is about 10%, and it is an amount of to get this product, 105 ℃ are dried to constant weight, take by weighing about 1.0g, and accurate the title decides, put in the porcelain dish, add sulfuric acid 6ml and nitric acid 10ml respectively, treat that 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, with hot wash 3 times, washing lotion filters residue in the lump, at last with on the residue dislocation filter paper with decantation, use hot wash, residue is waited to do silicon dioxide and is used; Filtrate 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, adding ammonia solution is neutralized to and just separates out precipitation, drip dilute sulfuric acid again and extremely precipitate till the just dissolving, add acetic acid-ammonium acetate buffer (pH6.0) 10ml, precision adds Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 3～5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, with zinc vs (0.05mol/L) titration, change redness into from yellow to solution, and titration results is proofreaied and correct with blank test.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is the Al203 of 2.549mg quite, calculates, and gets alundum (Al content 10.2%;
Get above-mentioned residue together with filter paper put with platinum alloy crucible in, drying, 800 ℃ blazing 2 hours down, put cold, accurate claim fixed.With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness, 800 ℃ blazing 5 minutes, put coldly, accurate claim surely, subtract the weight of mistake, be and contain SiO in the test sample
2Weight is calculated, and gets dioxide-containing silica 68.1%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, defective.
Embodiment 6
Get the diffusing bag of commercially available smectite, contain smectite 3g, add water 50ml, stir, filter 3 times repeatedly, remove auxiliary material, after the drying, be ground into fine powder, make X ray diffracting spectrum, carry out qualitative and quantitative analysis, smectite content is 95% as a result, contain a small amount of smalite in addition, α-cristobalite, it is an amount of to get this product, and 105 ℃ are dried to constant weight, take by weighing about 1.0g, the accurate title, decide, and puts in the porcelain dish, add sulfuric acid 6ml and nitric acid 10ml respectively, the effect for the treatment of fully, is put evaporate to dryness in the sand bath, puts cold, add dilute sulfuric acid 30ml, boil, upper strata liquid filters through ashless filter paper with decantation, and residue uses decantation with hot wash 3 times, washing lotion filters in the lump, with on the residue dislocation filter paper, use hot wash at last, residue is waited to do silicon dioxide and is used; Filtrate 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, adding ammonia solution is neutralized to and just separates out precipitation, drip dilute sulfuric acid again and extremely precipitate till the just dissolving, add acetic acid-ammonium acetate buffer (pH6.0) 10ml, precision adds Calcium Disodium Versenate vs (0.05mol/L) 25ml again, boiled 3～5 minutes, put and be chilled to room temperature, add xylenol orange indicator solution 1ml, with zinc vs (0.05mol/L) titration, change redness into from yellow to solution, and titration results is proofreaied and correct with blank test.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is the Al203 of 2.549mg quite, calculates, and gets alundum (Al content 57%;
Get above-mentioned residue together with filter paper put with platinum alloy crucible in, drying, 800 ℃ blazing 2 hours down, put cold, accurate claim fixed.With the residue water-wet, add 7 in hydrofluorite 7ml and sulfuric acid again, evaporate to dryness, 800 ℃ blazing 5 minutes, put coldly, accurate claim surely, subtract the weight of mistake, be and contain SiO in the test sample
2Weight is calculated, and gets dioxide-containing silica 20%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, qualified.
Embodiment 7
Get 6 of commercially available smectite dispersing tablets, contain smectite 3g, be ground into fine powder, make X ray diffracting spectrum, carry out qualitative and quantitative analysis, the result removes auxiliary material, smectite content is 97%, takes by weighing in right amount, and 105 ℃ are dried to constant weight, take by weighing about 0.25g, the accurate title, decide, and puts in the platinum crucible, be heated to 900 ℃, blazing 2 hours, cooling, add sulfuric acid 0.2ml and ethanol 2ml, make test sample moistening fully, add hydrofluorite 6ml, put 100 ℃ of-300 ℃ of evaporations, adding hydrofluorite 6ml when closely dried, continue to be evaporated to gas and eliminate, slowly be warming up to 900 ℃, blazing 1 hour, cooling, the accurate title, decide, the weight of twice blazing gained poor is and contains SiO in the test sample
2Amount, calculate, dioxide-containing silica 59.4%;
The preparation of alundum (Al reference substance solution: get Lu 1.0g, the accurate title, decide, and puts in the 1000ml measuring bottle, adds hydrochloric acid 10ml and water 10ml, after the dissolving, adds water to scale, shakes up, promptly;
The preparation of need testing solution: it is an amount of to get smectite, and 105 ℃ are dried to constant weight, take by weighing about 0.25g, the accurate title, decide, and puts in the platinum crucible, adds anhydrous lithium metaborate 1g, mix, slowly be warming up to 1100 ℃, blazing 15 minutes, put cold, crucible is placed the beaker of the rare nitric acid of 250ml (1 → 20), add rare nitric acid (1 → 20) 50ml again, Tianjin there is not crucible, crucible is put in the magnetic stirring, heating is stirred to dissolving fully, filters rapidly, filtrate is put in the 200ml measuring bottle, wash crucible and filter with water, washing lotion is incorporated in the measuring bottle, adds water to scale, shake up, promptly;
Measure alundum (Al content: precision is measured alundum (Al reference substance solution 0.5,1.0,2.0ml puts respectively in the 100ml measuring bottle, respectively add 1% sodium chloride solution 20ml, add water to scale, shake up, each reference substance solution and the need testing solution of dilution are shone atomic absorption spectrophotometry (two appendix IV of Chinese Pharmacopoeia version in 2005 D content determination, first method), measure at 309nm wavelength place, calculate, get alundum (Al content 16%.
Conclusion: this product is judged by silicon dioxide, alundum (Al content standard in the existing medicinal smectite content measuring standard, and is qualified.By standard determination of the present invention, qualified.
Claims (4)
1, medicinal smectite content measuring standard is characterized in that containing smectite and should be 95.0%-105.0%, presses dry product and calculates, and contains silicon dioxide (SiO
2) should be 55%-65%, trioxygen-containingization two aluminium (Al
2O
3) should be 12%-22%.
2, according to the medicinal smectite content measuring standard of claim 1, it is characterized in that the silicon dioxide content test method is gelatin method or hydrofluorite method, the alundum (Al content assaying method is titrimetry or atomic absorption spectrography (AAS).
3, according to the medicinal smectite content measuring standard of claim 1, it is characterized in that also can be used for the quality inspection of smectite preparation, get final product with smectite net content calculating in the smectite preparation.
4,, it is characterized in that the smectite preparation comprises powder, tablet, capsule, granule, supensoid agent, gel, the clinical formulation commonly used of dispersing tablet according to the medicinal smectite content measuring standard of claim 3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910014003XA CN101477068A (en) | 2009-01-20 | 2009-01-20 | Medicinal smectite content measuring standard |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102379894A (en) * | 2010-09-06 | 2012-03-21 | 济南康众医药科技开发有限公司 | Content determination method for montmorillonite preparation |
| CN102406657A (en) * | 2010-09-26 | 2012-04-11 | 济南康众医药科技开发有限公司 | Method for preparing montmorillonite preparation |
| CN102507484A (en) * | 2011-10-14 | 2012-06-20 | 济南康众医药科技开发有限公司 | Method for measuring content of zinc in compound montmorillonite preparation |
| CN102607985A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Water separation method for detecting impurity content and impurity categories of medicinal montmorillonite |
| CN105878275A (en) * | 2015-01-08 | 2016-08-24 | 许铨先 | Edible montmorillonite nanogel |
| CN106018447A (en) * | 2016-05-12 | 2016-10-12 | 济南康众医药科技开发有限公司 | Raw material selecting method for preparing medicine for reducing pesticide residues |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102379894A (en) * | 2010-09-06 | 2012-03-21 | 济南康众医药科技开发有限公司 | Content determination method for montmorillonite preparation |
| CN102379894B (en) * | 2010-09-06 | 2013-05-01 | 济南康众医药科技开发有限公司 | Content determination method for montmorillonite preparation |
| CN102406657A (en) * | 2010-09-26 | 2012-04-11 | 济南康众医药科技开发有限公司 | Method for preparing montmorillonite preparation |
| CN102406657B (en) * | 2010-09-26 | 2013-03-27 | 济南康众医药科技开发有限公司 | Preparation method of montmorillonite preparations |
| CN102507484A (en) * | 2011-10-14 | 2012-06-20 | 济南康众医药科技开发有限公司 | Method for measuring content of zinc in compound montmorillonite preparation |
| CN102607985A (en) * | 2012-03-06 | 2012-07-25 | 济南康众医药科技开发有限公司 | Water separation method for detecting impurity content and impurity categories of medicinal montmorillonite |
| CN105878275A (en) * | 2015-01-08 | 2016-08-24 | 许铨先 | Edible montmorillonite nanogel |
| CN106018447A (en) * | 2016-05-12 | 2016-10-12 | 济南康众医药科技开发有限公司 | Raw material selecting method for preparing medicine for reducing pesticide residues |
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