CN101126708A - Determination method and standard of montmorillonite for medicine and formulation adsorption force - Google Patents
Determination method and standard of montmorillonite for medicine and formulation adsorption force Download PDFInfo
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- CN101126708A CN101126708A CNA2007100148992A CN200710014899A CN101126708A CN 101126708 A CN101126708 A CN 101126708A CN A2007100148992 A CNA2007100148992 A CN A2007100148992A CN 200710014899 A CN200710014899 A CN 200710014899A CN 101126708 A CN101126708 A CN 101126708A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910052901 montmorillonite Inorganic materials 0.000 title abstract description 10
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000003814 drug Substances 0.000 title description 5
- 239000000203 mixture Substances 0.000 title description 2
- 238000009472 formulation Methods 0.000 title 1
- 238000001179 sorption measurement Methods 0.000 title 1
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 64
- 238000002360 preparation method Methods 0.000 claims abstract description 36
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 229910021647 smectite Inorganic materials 0.000 claims description 87
- 239000000243 solution Substances 0.000 claims description 84
- 238000010521 absorption reaction Methods 0.000 claims description 80
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 62
- 239000008363 phosphate buffer Substances 0.000 claims description 38
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 24
- 238000002835 absorbance Methods 0.000 claims description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 238000003556 assay Methods 0.000 claims description 19
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 18
- 238000004448 titration Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 229910019142 PO4 Inorganic materials 0.000 claims description 12
- 239000010452 phosphate Substances 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 238000002798 spectrophotometry method Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 9
- 229920002472 Starch Polymers 0.000 claims description 7
- 239000008107 starch Substances 0.000 claims description 7
- 235000019698 starch Nutrition 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000006210 lotion Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 6
- 239000012085 test solution Substances 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 239000002775 capsule Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000003826 tablet Substances 0.000 claims description 2
- 230000004962 physiological condition Effects 0.000 abstract description 4
- XQAXGZLFSSPBMK-UHFFFAOYSA-M [7-(dimethylamino)phenothiazin-3-ylidene]-dimethylazanium;chloride;trihydrate Chemical compound O.O.O.[Cl-].C1=CC(=[N+](C)C)C=C2SC3=CC(N(C)C)=CC=C3N=C21 XQAXGZLFSSPBMK-UHFFFAOYSA-M 0.000 abstract 3
- 239000000463 material Substances 0.000 description 15
- 230000000694 effects Effects 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- QMGVPVSNSZLJIA-UHFFFAOYSA-N Nux Vomica Natural products C1C2C3C4N(C=5C6=CC=CC=5)C(=O)CC3OCC=C2CN2C1C46CC2 QMGVPVSNSZLJIA-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000005341 cation exchange Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- QMGVPVSNSZLJIA-FVWCLLPLSA-N strychnine Chemical compound O([C@H]1CC(N([C@H]2[C@H]1[C@H]1C3)C=4C5=CC=CC=4)=O)CC=C1CN1[C@@H]3[C@]25CC1 QMGVPVSNSZLJIA-FVWCLLPLSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 241001279009 Strychnos toxifera Species 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 238000004166 bioassay Methods 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 125000001475 halogen functional group Chemical group 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229940085605 saccharin sodium Drugs 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 229960005453 strychnine Drugs 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 241000256844 Apis mellifera Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 150000001768 cations Chemical class 0.000 description 1
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- 229920002678 cellulose Polymers 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- -1 metallurgy Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000003969 polarography Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 239000004576 sand Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Medicinal Preparation (AREA)
Abstract
The utility model relates to a determination method of a medicinal montmorillonite and the absorbability of the preparation, which is to determine the montmorillonite and the absorbability of the preparation by methylene blue with the testing standard that 0.23 to 0.48g methylene blue (C16H18ClN3S) is absorbed by every 1g montmorillonite or the preparation containing 1g montmorillonite. The utility model has the advantages of accurate reflection of the absorbability of medicinal montmorillonite under physiological conditions, accurate and reliable result and more effective control.
Description
Invention field
The present invention relates to a kind of medicine detection method, the particularly a kind of method of smectite and preparation absorption affinity and standard of mensuration measured.
Background of invention
Smectite looses as a kind of mucosa protective agent efficiently, and the adsorbent of germ, virus and toxin thereof is used for the treatment of various acute and chronic diarrhoeal diseases, high effect nontoxic, now more than 100 countries and regions listing in the whole world.
Smectite (montmorillonite), claim montmorillenite or glue mountain range soil again, be under the jurisdiction of the dioctahedron subtribe in the smectite family, be a kind of hydrated silicate mineral of complicated component, liquid water content changes greatly, be the main composition of bentonitic clay (bentinite) and bleaching earth (bleaching earth), its molecular formula generally is expressed as (Al
33-1.67Mg
0.33_0.67) (Ca
0-1Na
0-1)
0.33Si
4(OH)
2O
10XH
2O, also can be expressed as simply (Na, Ca)
0.33(Al, Mg)
2(Si
4O
10) (OH)
2NH
2O.Be the dioctahedron of symmetry on the smectite space structure, be lamellar under the scanning electron microscope.Inner structure is because Al
3+To some extent by Mg
2+, Ca
2+Deng replacement, cause the imbalance of internal charge, three charge-sites of corresponding formation, promptly in the layer, interlayer and layer end, its middle level in and the charged negativity of interlayer, and layer is held positively charged, and the particle diameter of smectite is less than 2 μ m, and its specific surface area is greater than 100m
2/ g.These particular structure make it have the absorption and the gelling of height just, are widely used in fields such as building materials, metallurgy, oil, chemical industry, agricultural, medicine, machinery, light industry, food, environmental protection.
The absorption affinity of smectite derives from the imbalance of its internal charge.In the smectite Si-O tetrahedral sheet, the Si of tetravalence is replaced by the Al of trivalent sometimes, in the Al-O octahedral sheet, the Al of trivalent is replaced by the Mg of divalence sometimes, and this just causes the positive charge deficiency, the negative charge surplus, the negative charge of this surplus is compensated by the kation of absorption on the crystal layer surface, and when having water to exist, the compensating cation on crystal layer surface is easily by other cation exchange, be called exchange absorption, this exchange absorption is equivalent absorption.
The absorption affinity of medicinal smectite is the pharmacological basis of its absorbing pathogenic bacteria, virus and bacteriotoxin effect, and the mensuration of absorption affinity is an important indicator of control smectite quality.Accurately detecting the smectite absorption affinity is effectively to control the method that product quality is guaranteed curative effect.The method that detects the smectite absorption affinity in the existing national drug standards is to use spectrophotometric method, measures the amount of absorption sulfuric acid strychnine.It is more accurate that this method is measured absorption affinity, but the sulfuric acid strychnine belongs to toxic articles, and it is very inconvenient to buy, manage, use, and the price height, and expense is big.
Blue amount is inhaled by detecting the ability of smectite absorption methylene blue, being called for short in other field, determines the content of smectite in the material, has obtained using more widely.By measuring the content of smectite in the casting sand, can improve the condition of casting, and then improve the quality of foundry goods.According to analysis to smectite content in the oil drilling mud, suitably adjust the ratio of mud, can improve the efficient of drilling well.In addition, in geologic prospecting,, also be a kind of simple universal method with the content of inhaling smectite in the blue amount method geodetic layer.
Owing to determine to inhale the method difference of blue quantitative response terminal point, it is also different to measure the used method of the blue amount of suction.From the article of having reported, mainly contain the halo method (Zhang Naixian is etc. clay mineral science study method. Science Press, 1990,183); Oscilloscopic polarography (Ye Huali, etc. analytical chemistry, 1986,14 (12): 928); Spectrophotometric method (L.ScderLing, et al.AFS Transactions, 1983,91:77).
The halo method is easy to operate, instrument is simple, uses the most general.Because repeatedly get drop on test paper, will observe the terminal point of determining of green ring simultaneously with eyes, the size of green ring is bigger because of people's judgement difference, and terminal point determining is to get liquid to observe simultaneously, cause resultant error bigger, the accuracy of method and precision all are restricted.
The terminal point that oscillopolarographic detection is inhaled blue quantitative response is more accurate, but the instrument more complicated because of using is restricted the widespread use of this method.
The step of the spectrophotometric method of having reported is, sample is added distilled water to be shaken, sample is fully scattered in water, adding 1% sodium pyrophosphate solution again shakes up, the conical flask that fills mixed solution is placed little the boiling 5 minutes of heating on the electric furnace, make ca-montmorillonite change sodium base shape into, and make it high degree of dispersion.Allow excessive methylene blue fully be adsorbed, survey the absorbance that the remaining methylene blue of solution is produced again, and then check in the content of smectite from the typical curve of being done by standard smectite sample by sample.What this method detected is the content of smectite, is not to survey the blue amount of inhaling.This method also can calculate inhales blue amount, but uses sodium pyrophosphate solution in the method, heats little boiling, and makes ca-montmorillonite change sodium base shape into, and makes it high degree of dispersion, measures absorption affinity then.If the absorption affinity with this method mensuration medicinal smectite can not accurately truly reflect the absorption affinity of medicinal smectite under physiological condition; Little the boiling 5 minutes of this method heating has water evaporates in the heating process, make the result inaccurate; The methylene blue reagent purity that this method is used is 97%, and solution is joined not through demarcating by institute, and methylene blue solution concentration is inaccurate, also makes the result inaccurate.Therefore, can not effectively control product quality, guarantee the curative effect of medicinal smectite;
Summary of the invention
The object of the present invention is to provide a kind of new, do not use the sulfuric acid strychnine, can truly reflect medicinal smectite and the absorption affinity of preparation under physiological condition, effectively control product quality, guarantee the medicinal smectite curative effect, accurately detect the assay method of medicinal smectite absorption affinity.
Another object of the present invention provides a kind of bioassay standard that detects medicinal smectite and preparation absorption affinity.
The objective of the invention is to be achieved through the following technical solutions:
At first demarcate methylene blue solution, it is an amount of to get smectite, quantitatively add phosphate buffer, shake well disperses, quantitatively add the methylene blue standard solution again, allow excessive methylene blue fully be adsorbed, use the remaining methylene blue of spectrophotometry solution again, calculate the absorption affinity of smectite then by sample.
Determination step
(1) the preparation massfraction is 0.2% methylene blue solution: be taken at 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.00g, the water solution transfer is to the brown volumetric flask of 1000ml, and thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put and be heated to 75 ℃ in the water-bath, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S.
(2) preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, regulate pH to 6.8 ± 0.05 with 2mol/L hydrochloric acid solution or 2mol/L NaOH in case of necessity.
(3) absorption affinity assay method: get the about 0.200g of smectite, the accurate title, decide, put in the tool plug conical flask, accurate phosphate buffer (pH6.8) 10ml that adds, jolting 1 hour, placed 24 hours, the accurate methylene blue mark solution 50ml that adds puts in 37 ℃ of water-baths, jolting 1 hour, middling speed filter paper with drying filters, and precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, add phosphate buffer (pH6.8) and be diluted to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, add phosphate and be diluted to scale towards liquid (pH6.8), shake up, make need testing solution, according to spectrophotometric method (two appendix IVA of Chinese Pharmacopoeia version in 2005), absorbance log is measured in selecting as measuring wavelength between 660nm and 670nm: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and make the solution that contains 2ug among every ml, compare solution, measure absorbance log, calculate absorption affinity according to following formula with method.
A
1: the contrast solution absorbance log
A
2: the need testing solution absorbance log
C:0.2% methylene blue concentration of standard solution
M: the smectite amount of taking by weighing
D:0.2% methylene blue titer extension rate
The present invention preferably measures wavelength 665nm place according to spectrophotometric method.
Smectite has ion exchangeable, the kation of smectite is exchanged by the methylenum careuleum equivalent, smectite cation exchange capacity (CEC) 70-150 milligramequivalent/100g, methylenum careuleum (C16H18C1N3S) molecular weight 325.9, gram equivalent is 325.9, calculate with smectite cation exchange capacity (CEC) 70-150 milligramequivalent/100g, the amount of smectite absorption methylenum careuleum (C16H18C1N3S) is between 0.228-0.489g/g.Examination criteria is decided to be 0.23-0.48g/g.
The assay method of medicinal smectite absorption affinity of the present invention can be used for smectite raw material and smectite preparation.The smectite preparation comprises clinical acceptable forms such as powder, tablet, capsule, granule, supensoid agent, gel, dispersing tablet.
The assay method of medicinal smectite absorption affinity of the present invention with the weight of spectrophotometry absorption methylene blue, thereby has been avoided use toxic articles sulfuric acid strychnine, purchase, management, easy to use, and price is low, saves laboratory fee and uses.The present invention has also improved other field perfect and has detected the method for smectite absorption methylene blue amount, do not use sodium pyrophosphate solution, do not heat little boiling, do not make ca-montmorillonite change sodium base shape into, and make it high degree of dispersion, and use the phosphate buffer in two appendix I of Chinese Pharmacopoeia version in 2005 D, second method, can accurately reflect the absorption affinity of medicinal smectite under physiological condition, effectively control product quality, guarantee the curative effect of medicinal smectite.
The assay method of below routine by experiment further proof medicinal smectite absorption affinity of the present invention, good stability, accuracy height.
The research of experimental example 1 medicinal smectite absorption affinity assay method
1, instrument and medicine
Ultraviolet-visible pectrophotometer (the general all purpose instrument company limited of analysing in TU-1800 Beijing)
Ph counts (phs-3c Shanghai thunder magnetic)
Methylene blue (biological stain, Shanghai reagent three factories);
Smectite (lot number: 20060612, Hainan Xiansheng Pharmaceutical Co., Ltd)
2, experiment and result
2.1 the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.00g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put in the water-bath and heat 75 ℃, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S.
The concentration that calculates methylene blue solution is: 0.201%
2.2 preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, get pH value 6.8 with the Ph instrumentation.
2.3 the preparation of need testing solution: get smectite 0.2006g, put in the Erlenmeyer flask accurate adding phosphate buffer (pH6.8) 10ml, jolting 1 hour, placed 24 hours, precision adds methylene blue solution 10ml, and jolting is 1 hour in 37 ℃ of water-baths, and is centrifugal, precision is measured supernatant 10ml, put in the 250ml measuring bottle, add phosphate buffer (PH6.8) and be diluted to scale, shake up.The accurate 5ml that draws puts in the 50ml measuring bottle, adds above-mentioned damping fluid and is diluted to scale, shakes up.As need testing solution.
2.4 describing of ultraviolet absorption curve.
Describing of methylene blue solution ultraviolet absorption curve: get methylene blue solution and add phosphate buffer and make the solution that every 1ml contains 2 μ g, with the phosphate buffer is blank, on ultraviolet spectrophotometer,, record ultraviolet absorption curve in the interscan of 550-750nm wavelength coverage.
Describing of test sample ultraviolet absorption curve: getting need testing solution, is blank with the phosphate-buffered, in the interscan of 550-750nm wavelength coverage, records ultraviolet absorption curve on ultraviolet spectrophotometer.
Compare methylene blue solution ultraviolet absorption curve and test sample ultraviolet absorption curve as can be seen, the ultraviolet absorption curve and the maximum absorption wavelength of test sample and reference substance are in full accord; Methylene blue is in 660～670nm wavelength coverage, bigger absorbance is arranged, and absorb honeybee and be in-flat condition, maximum absorption wavelength is 665nm, promptly absorbance remains unchanged substantially when wavelength variations, so select the point between 660nm and the 670nm all can as measuring wavelength.The preferred 665nm of the present invention, promptly ensuring method has enough sensitivity, can reduce the influence of wavelength selection to measurement result again.
2.5 absorbance log and concentration linear relationship are investigated
Get methylene blue titer (0.18%), precision is measured 2ml and is put in the 100ml measuring bottle.Add phosphate buffer (pH6.8) and be diluted to scale, shake up, accurate respectively absorption 0.5,1.0,1.5,2.0,2.5,3.0,3.5,4.0,5.0,6.0ml respectively put in the 50ml measuring bottle, and add phosphate buffer (pH6.8) and be diluted to scale, shake up and make linear solution.Measure absorbance log at 665nm wavelength place.The results are shown in Table 1
Table 1 linear relationship test findings
| Concentration (μ g/ml) | 0.36 | 0.72 | 1.08 | 1.44 | 1.80 | 2.16 | 2.88 | 3.60 | 4.32 |
| Absorbance log | 0.084 | 0.165 | 0.249 | 0.347 | 0.431 | 0.523 | 0.708 | 0.873 | 1.069 |
Getting regression equation is: y=0.2475x-0.0094, r=0.9997.
Experiment shows that methylene blue is good in 0.36～4.32 μ g/ml concentration range internal linear relation.
2.6 the investigation of precision.
Get methylene blue titer (0.18%), be configured to the solution to be measured of 2.16 μ g/ml, and the photograph spectrophotometric method " two appendix IVA of Chinese pharmacopoeia version in 2005), measure absorbance log, repetitive operation 6 times at 665nm wavelength place.The results are shown in Table 2
Table 2 Precision test result
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 | RSD(％) |
| Absorbance log | 0.524 | 0.524 | 0.524 | 0.524 | 0.523 | 0.524 | 0.08 |
By the result as can be known under this test condition precision good.The result shows, this experiment precision height, and method is reliable.
2.7 repeatability
Get each about 0.200g of 6 duplicate samples, the accurate title, decide, and according to " preparation of need testing solution " method, makes solution to be measured.The place measures absorbance log respectively at the 665nm wavelength, calculates absorption affinity. the results are shown in Table 3:
Table 3 replica test result
| Numbering | Absorption affinity (g/g) | Average absorption affinity (g/g) | RSD(％) |
| 1 2 3 4 5 6 | 0.336 0.334 0.330 0.335 0.331 0.337 | 0.334 | 0.83 |
The result shows that it is good that this method is measured methylene blue absorption affinity repeatability.
2.8 study on the stability is got " replica test " item a need testing solution down, places 8 hours in room temperature, every sampling in 2 hours, measures absorbance log at 665nm wavelength place, test findings sees Table 4:
Table 4 solution stability testing result
| Time | 0 hour | 2 hours | 4 hours | 6 hours | 8 hours | RSD％ |
| Absorbance log | 0.367 | 0.368 | 0.368 | 0.368 | 0.369 | 0.2 |
The result shows that solution is stable in 8 hours
The mensuration of experimental example 2 smectites and preparation absorption affinity
According to 10 batches of smectites of assay method mensuration of above-mentioned absorption affinity and the absorption affinity of preparation, measurement result sees the following form
| Kind | Lot number | Absorption affinity (g/g) |
| The diffusing smectite of the diffusing smectite of the diffusing smectite of the diffusing smectite of smectite smectite smectite smectite mixes the mixed liquid smectite dispersing tablet of liquid smectite | 060901 070101 070202 061201 070302 070203 060804 060501 070802 050301 | 0.25 0.35 0.48 0.32 0.41 0.27 0.28 0.36 0.33 0.34 |
Record smectite and preparation absorption affinity between 0.25-0.48, and calculate according to smectite cation exchange capacity (CEC), therefore the examination criteria that obtains is 0.23-0.48g/g.
Embodiment
Embodiment 1 smectite absorption affinity assay method
1, the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.0611g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put in the water-bath and heat 75 ℃, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S.
The concentration that calculates methylene blue solution is: 0.201%
2, preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, get pH value 6.83 with the Ph instrumentation.
3, get smectite 0.19961g, put in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds, jolting 1 hour, placed 24 hours, the accurate methylene blue mark solution 50ml that adds puts in 37 ℃ of water-baths, jolting 1 hour, middling speed filter paper with drying filters, and precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, add phosphate buffer (pH6.8) and be diluted to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, add phosphate and be diluted to scale towards liquid (pH6.8), shake up, according to spectrophotometric method (two appendix IVA of Chinese Pharmacopoeia version in 2005), measure absorbance log at 665nm wavelength place: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and make the solution that contains 2ug among every ml, measure absorbance log with method, calculate.The amount of every gram smectite absorption methylene blue is 0.333g.
The embodiment 2 smectites absorption affinity assay method that looses
Prescription: every bag contains smectite 3g, glucose 0.749g, saccharin sodium 0.007g, vanillic aldehyde 0.004g.
Lot number: 20060306
1, the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.01g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put in the water-bath and heat 75 ℃, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S.
The concentration that calculates methylene blue solution is: 0.199%
2, preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, get pH value 6.83 with the Ph instrumentation.
3, auxiliary material is tested the influence of absorption affinity mensuration: getting auxiliary material in the prescription ratio, get the auxiliary material of 0.06g mixing, add in the phosphate buffer and dissolve, is blank with the phosphate buffer, and in the scanning of 550-750nm wavelength coverage, auxiliary material is in the nothing absorption of 665nm place as a result.
Getting methylene blue solution adds phosphate buffer and makes the solution that every 1ml contains 2 μ g, the auxiliary material dissolving that adds the 0.06g mixing, with the phosphate buffer is blank, on ultraviolet spectrophotometer in the interscan of 550-750nm wavelength coverage, record ultraviolet absorption curve, the presentation of results auxiliary material does not disturb the absorption curve of methylene blue.
Two test explanation auxiliary materials are measured absorption affinity does not have influence.
Absorption affinity is measured: precision takes by weighing the diffusing 0.250g (being equivalent to smectite 0.200g approximately) of smectite, put in the tool plug conical flask, accurate phosphate buffer (pH6.8) 10ml that adds, jolting 1 hour, placed 24 hours, the accurate methylene blue mark solution 50ml that adds puts in 37 ℃ of water-baths, jolting 1 hour, middling speed filter paper with drying filters, and precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, add phosphate buffer (pH6.8) and be diluted to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, add phosphate and be diluted to scale towards liquid (pH6.8), shake up, according to spectrophotometric method (two appendix IVA of Chinese Pharmacopoeia version in 2005), measure absorbance log at 665nm wavelength place: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and make the solution that contains 2ug among every ml, measure absorbance log with method, calculate.The amount of every gram smectite absorption methylene blue is 0.308g.
Embodiment 3 smectite dispersing tablet absorption affinity assay methods
Prescription: per 1000 contain smectite 1000g, glucose 7g, saccharin sodium 3g, vanillic aldehyde 4g, little smart cellulose 100g, sodium carboxymethyl starch 30g.
Lot number: 20070203
1, the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.02g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put in the water-bath and heat 75 ℃, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S.
The concentration that calculates methylene blue solution is: 0.192%
2, preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, get pH value 6.81 with the Ph instrumentation.
3, auxiliary material is tested the influence of absorption affinity mensuration: getting auxiliary material in the prescription ratio, get the auxiliary material of 0.06g mixing, add in the phosphate buffer and dissolve, is blank with the phosphate buffer, and in the scanning of 550-750nm wavelength coverage, auxiliary material is in the nothing absorption of 665nm place as a result.
Getting methylene blue solution adds phosphate buffer and makes the solution that every 1ml contains 20 μ g, the auxiliary material dissolving that adds the 0.06g mixing, with the phosphate buffer is blank, on ultraviolet spectrophotometer in the interscan of 550-750nm wavelength coverage, record ultraviolet absorption curve, the presentation of results auxiliary material does not disturb the absorption curve of methylene blue.
Two test explanation auxiliary materials are measured absorption affinity does not have influence
Absorption affinity is measured: get smectite dispersing tablet porphyrize, precision takes by weighing fine powder 0.255g and puts in the tool plug conical flask, accurate phosphate buffer (pH6.8) 10ml that adds, jolting 1 hour, placed 24 hours, the accurate 0.2% methylene blue mark solution 50ml that adds puts in 37 ℃ of water-baths, jolting 1 hour, middling speed filter paper with drying filters, and precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, add phosphate buffer (pH6.8) and be diluted to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, add phosphate and be diluted to scale towards liquid (pH6.8), shake up, according to spectrophotometric method (two appendix IVA of Chinese Pharmacopoeia version in 2005), measure absorbance log at 665nm wavelength place: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and make the solution that contains 2ug among every ml, measure absorbance log with method, calculate.The amount of every gram smectite absorption methylene blue is 0.35g.
Claims (7)
1. the assay method of medicinal smectite and preparation absorption affinity is characterized in that may further comprise the steps:
(1) the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.00g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 24h.Precision is measured this liquid 50ml, put in the water-bath and heat 75 ℃, precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up, 75 ℃ of insulations 20 minutes, put cold, filter with sintered glass funnel, beaker and funnel wash with water 4 times, each 2.5ml, filter, merging filtrate and washing lotion in the dislocation tool plug conical flask, add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml, shake up, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C of 10.66mg
16H
18ClN
3S;
(2) preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixed by 3: 1, regulate pH to 6.8 ± 0.05 with 2mol/L hydrochloric acid solution or 2mol/L NaOH in case of necessity;
(3) absorption affinity assay method: get the about 0.200g of smectite or contain the smectite preparation of the about 0.200g of smectite, the accurate title, decide, put in the tool plug conical flask, accurate phosphate buffer (pH6.8) 10ml that adds, jolting 1 hour, placed 24 hours, the accurate methylene blue mark solution 50ml that adds, put in 37 ℃ of water-baths, jolting 1 hour filters with dry middling speed filter paper, precision is measured subsequent filtrate 10ml, put in the 250ml measuring bottle, add phosphate buffer (pH6.8) and be diluted to scale, shake up, precision is measured 5ml, put in the 50ml measuring bottle, add phosphate and be diluted to scale, shake up towards liquid (pH6.8), according to spectrophotometric method (two appendix IV of Chinese Pharmacopoeia version in 2005 A), selecting between 660-670nm wavelength place measured absorbance log: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and make the solution that contains 2ug among every ml, measures absorbance log with method, calculates.Every 1g smectite or the preparation that contains the 1g smectite should adsorb methylene blue (C
16H
18ClN
3S) 0.23-0.48g.
2. the assay method of medicinal smectite as claimed in claim 1 and preparation absorption affinity is characterized in that measuring medicinal smectite and preparation absorption affinity with methylene blue.
3. the assay method of medicinal smectite as claimed in claim 1 and preparation absorption affinity is characterized in that methylene blue is mixed with titer and measures medicinal smectite and preparation absorption affinity.
4. the assay method of medicinal smectite as claimed in claim 1 and preparation absorption affinity is characterized in that using phosphate buffer (pH6.8) with its dispersion, adds the methylene blue titer, after waiting to adsorb, measures the residue methylene blue, calculates the methylene blue adsorbance.
5. the assay method of medicinal smectite absorption affinity as claimed in claim 1 is characterized in that detecting wavelength and selects point between 650nm and the 670nm as measuring wavelength.
6. the assay method of medicinal smectite absorption affinity as claimed in claim 5 is characterized in that detecting wavelength and is preferably 650nm.
7. the assay method of medicinal smectite as claimed in claim 1 and preparation absorption affinity is characterized in that the smectite preparation comprises clinical acceptable forms such as powder, tablet, capsule, granule, supensoid agent, gel, dispersing tablet.
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| 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 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4047738A (en) * | 1976-01-12 | 1977-09-13 | Engelhard Minerals & Chemicals Corporation | Record sheets sensitized with reduced charge montmorillonite pigment |
| JPS6110020A (en) * | 1984-06-22 | 1986-01-17 | Mizusawa Ind Chem Ltd | Synthetic lamellar magnesium phyllosilicate and its preparation |
| US5130028A (en) * | 1990-09-17 | 1992-07-14 | Rheox, Inc. | Method of treating waste water for organic contaminants with water dispersible organically modified smectite clay compositions |
| JP2006213588A (en) * | 2005-02-02 | 2006-08-17 | Minoru Shiromizu | Viscous titanium oxide and method for forming film of the same |
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- 2007-09-17 CN CNB2007100148992A patent/CN100516831C/en active Active
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